Microfabrication apparatus

Abstract

To provide a micronization treatment apparatus capable of performing micronization treatment of slurry fluid in which viscosity of suspension fluid is high or a solid content, a fiber, and a powder are included, and capable of suppressing facility damage or the like due to pulsation of high-pressure suspension fluid, and to provide a micronization treatment apparatus capable of suppressing an energy consumption unit required for the micronization treatment, and capable of reducing costs by reducing the number of times of the micronization treatment.SOLUTION: A micronization treatment apparatus includes a raw material tank, a raw material supply pump, a raw material discharge pipe, a raw material suction pipe, a raw material return pipe, and / or a raw material circulation pipe, a crank-driven pressure type booster, and a chamber including micronization treatment means, where the raw material supply pump and the raw material suction pipe are for pressurizing and supplying raw material to the booster, and the raw material circulation pipe and the raw material return pipe are for returning the raw material to the raw material tank.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a miniaturization processing apparatus.

Background Art

[0002] In various fields such as electronic components, chemical materials, food, pharmaceuticals, and chemistry, a miniaturization processing apparatus for miniaturizing various substances such as metal particles and plant fibers is used. This miniaturization processing apparatus generally includes a discharge means such as a plunger pump that applies a high pressure to a suspension fluid, and a miniaturization processing means such as a miniaturization nozzle or a miniaturization flow path that miniaturizes the substances contained in the suspension fluid.

[0003] Patent Document 1 discloses that the discharge means of the collision device needs to be selected according to the presence or absence of solid matter to be miniaturized. Specifically, when the raw material liquid is a slurry liquid containing solid matter, from the viewpoint of the durability of the device so that the pump is not damaged by the solid matter, it is suitable to employ a hydraulic booster type ultra-high pressure pump that can move the plunger slowly, and when the raw material liquid does not contain solid matter, since it is not necessary to use a hydraulic device that can operate the plunger slowly, it is disclosed that a crank type plunger pump that rotates a crankshaft by an electric motor and converts it into a reciprocating motion to operate the plunger is suitable.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] However, the sliding speed of the cylinder head of the hydraulic booster type ultra-high pressure pump described in Patent Document 1 is low, with a speed of several seconds for one reciprocation. In the case of continuous fine processing on an industrial scale when the raw material liquid is a slurry liquid containing solids, it was essential to use a combination of multiple hydraulic booster type ultra-high pressure pumps. Therefore, since the high-pressure suspension fluid is discharged from each hydraulic booster type ultra-high pressure pump at intervals of several seconds alternately, the pressure fluctuation range of the discharged high-pressure suspension fluid was large. To control these movements, the introduction of proportional valves, servo motors, etc. was required. Due to this pressure fluctuation, there were several problems such as damage inside the ultra-high pressure components and breakage due to deterioration, and wear of the seal components of the cylinder head that slides at a low speed. Also, generally, since the hydraulic booster type ultra-high pressure pump is large-sized, the entire fine processing apparatus including this pump becomes large-sized, requiring a large installation area and resulting in high introduction costs.

[0006] On the other hand, in the case of a slurry fluid with a high viscosity of the suspension fluid or containing solids, fibers, or powders, if a crank type plunger pump is adopted, since the plunger driving speed of the crank type plunger pump is high, when sucking in the raw material, poor suction of the raw material liquid due to its viscosity, sedimentation separation, aggregation, etc. may occur, causing the inside of the cylinder to become a vacuum state, and there was a risk of an explosion caused by the Diesel effect during negative pressure.

[0007] Therefore, in view of the above problems, the present invention provides a fine processing apparatus capable of finely processing a suspension fluid (hereinafter sometimes referred to as a suspension fluid) with a high viscosity or containing solids, fibers, or powders, and suppressing equipment damage and the like caused by the pulsation of the high-pressure suspension fluid.

[0008] Another object of the present invention is to reduce the energy unit required for the micronization process, further stabilize the pressure fluctuation range of the high-pressure suspension fluid discharged, and perform reliable micronization processing with a stable ultra-high pressure flow to reduce the number of micronization processes and provide a micronization processing apparatus capable of cost reduction.

Means for Solving the Problems

[0009] As a result of intensive studies to achieve the above object, the inventors of the present invention, even when performing micronization processing of a suspension, set the driving method of the booster to a crankshaft method with a fast reciprocating speed of the plunger, making the movement of the plunger regular and periodic at high speed, and increasing the discharge pressure of the raw material supply pump to stably supply the suspension fluid to the booster, thereby suppressing the fluid pressure fluctuation of the suspension fluid and increasing the amount of micronization processing per unit time.

[0010] That is, the present invention is a micronization processing apparatus including a raw material tank, a raw material supply pump, a raw material discharge pipe, a raw material suction pipe, a raw material return pipe and / or a raw material circulation pipe, a booster, and a chamber provided with micronization processing means, wherein the raw material supply pump and the raw material suction pipe are for pressurizing and supplying the raw material to the booster, and the raw material circulation pipe and the raw material return pipe are for returning the surplus while maintaining the pressure of the pressurized raw material at a high level to the raw material tank.

Effects of the Invention

[0011] According to the micronization processing apparatus of the present invention, there is provided a micronization processing apparatus capable of micronization processing of a suspension fluid having a high viscosity or a slurry fluid containing solid components, fibers, or powders, and suppressing equipment damage due to pulsation of the high-pressure suspension fluid. In addition, there is provided a micronization processing apparatus capable of suppressing the energy unit required for the micronization process and further reducing costs by reducing the number of micronization processes.

Brief Description of the Drawings

[0012]

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Figure 6

Figure 7

Mode for Carrying Out the Invention

[0013] Hereinafter, the micronization processing apparatus according to the present invention will be described in detail. However, the following embodiments are for helping the understanding of the invention and do not limit the present invention.

[0014] (Definition of Terms) The "raw material" in this specification refers to what is used as the raw material for micronization processing, and is used for a slurry liquid having a high viscosity containing such a raw material, or a slurry liquid containing solid content, fiber, or powder. The term "micronization processing" in this specification means performing some physical treatment on a raw material brought to a high-pressure state using a booster. The "processing liquid" in this specification refers to the liquid after performing micronization processing on the raw material. In other words, it refers to the raw material liquid that has passed through this micronization processing apparatus one or more times.

[0015] As shown in FIG. 1, the micronization processing apparatus 1 of this embodiment mainly includes a raw material tank 2 for storing raw materials, a raw material supply pump 4, a raw material discharge pipe 3, a raw material circulation pipe 5, a raw material suction pipe 6, a raw material return pipe 7, a booster 8, a chamber 10, a processing liquid tank 13, and a processing liquid return pipe 18.

[0016] The raw material tank 2 is supplied with and stores raw materials. Various known stirring devices 23 may be attached to the raw material tank to stir the raw materials. The suction port of the raw material supply pump 4 is connected to this raw material tank 2 via the raw material discharge pipe 3.

[0017] Examples of the raw materials include starch powder, polyvinyl alcohol powder, and dissolved cellulose powder, which have poor solubility, tend to form lumps, and become highly viscous solutions. Also included are cellulose fibers derived from polysaccharides containing natural plants such as wood fibers, bamboo fibers, sugarcane fibers, seed hair fibers, and leaf fibers that require refinement, or those obtained by chemically modifying these. As other raw materials, those used in the chemical industry, such as toner dispersion, preparation of aqueous paints, wet dispersion and crushing of organic and inorganic powders and colored pigment powders, and those used in the electronic component industry, such as wet dispersion and crushing of organic and inorganic powders, can be used as appropriate without particular limitation. It is particularly suitable for raw materials whose viscosity increases due to refinement.

[0018] Also, as a pretreatment for performing the refinement treatment described later, those obtained by chemically modifying raw materials such as pulp can also be used as raw materials in this embodiment. Examples include hydrolysis of polysaccharides by acids, hydrolysis of polysaccharides by enzymes, swelling of polysaccharides by alkalis, oxidation of polysaccharides by oxidizing agents, reduction of polysaccharides by reducing agents, oxidation by TEMPO catalysts, phosphorylation, carbamation, cationization, etc.

[0019] The raw material supply pump 4 is preferably a pump that can send the solid matter in the suspension without biting it and can send the liquid even when the viscosity increases. A positive displacement metering pump is preferred. Among positive displacement metering pumps, non-contact pumps are preferred from the perspective of preventing foreign matters such as contaminated powder from clogging the injection nozzle. In particular, bead pumps, tube pumps, and twin screw pumps are preferred. Also, it is preferable to use those having a performance with an upper limit value of the discharge pressure of various positive displacement metering pumps in the range of 0.2 MPa to 10 MPa. Furthermore, by setting the discharge pressure of various volumetric metering pumps to at least 0.2 MPa, preferably 0.3 MPa, and more preferably 0.4 MPa or higher, it becomes possible to prevent poor suction of the raw material liquid.

[0020] In addition, a raw material suction pipe 6, a raw material circulation pipe 5, and a pressure regulating valve (not shown) are connected to the raw material supply pump 4. Furthermore, a switching valve (not shown) or the like can be provided in the raw material circulation pipe 5 and the raw material suction pipe 6 so that liquid can be sent to either one of them. By connecting in this way, the suspension fluid can be circulated between the booster pump 8 and the raw material tank 2. When using in this way, although not shown, the pressure regulating valve may be attached to the raw material circulation pipe 5 or the raw material return pipe 7, and it may be operated only with the raw material return pipe 7 without using the raw material circulation pipe 5. By doing so, the location where the raw material stays can be reduced, and the circulation can be performed more smoothly.

[0021] By installing a pressure regulating valve (not shown), the pressure on the inlet side of the booster pump can be made constant, and the operability of the miniaturization treatment apparatus according to the present invention is stabilized. In addition, by monitoring the valve opening degree, abnormalities can be detected at an early stage. For example, if the nozzle is blocked, the valve opening degree increases, and if the inside of the nozzle is worn, the valve opening degree tends to decrease.

[0022] A product recovery pipe 21 for recovering the product after performing the miniaturization treatment a specified number of times is connected to the raw material circulation pipe 5, and a product tank 22 is connected to the product recovery tank 21. Although not shown, the product recovery pipe 21 may be connected to the cooler 17 to take out the product from the cooler, or of course, it may be taken out from the chamber outlet pipe 12. In that case, the product can be obtained at a high temperature.

[0023] The chamber 10 is provided with miniaturization treatment means for performing miniaturization treatment inside the chamber. Examples of the miniaturization treatment means include means for performing miniaturization treatment by physical methods such as shear force, cavitation, collision against a hard body for collision such as impact ring, or mutual collision of high-pressure jets due to changes in pressure and speed.

[0024] Hereinafter, the case where the atomization treatment is performed using a high-pressure injection nozzle as the atomization treatment means will be described. A high-pressure injection nozzle 11 extending and connected from the chamber supply ultra-high pressure pipe 9 is connected to the chamber 10, and the atomization treatment of the raw material is performed in the chamber 10. Further, in the chamber 10, the chamber outlet pipe 12, the treatment liquid tank 13, the treatment liquid discharge pipe 14, the treatment liquid return pump 15, the cooler feed pipe 16, the cooler 17, and the treatment liquid return pipe 18 can be connected according to the number of atomization treatments. By providing the treatment liquid tank 13, the treatment liquid discharge pipe 14, and the treatment liquid return pump 15, the cooler 17 can be a high-efficiency type cooler with pressure applied. In addition, since the exhaust pressure at the chamber outlet can be set to atmospheric pressure, the pressure difference on the nozzle outlet side becomes larger, so that the atomization treatment efficiency can also be increased.

[0025] The chamber outlet pipe 12 is used to take out the liquid after the raw material has been atomized one or more times by the high-pressure injection nozzle 11 in the chamber 10 and store it in the treatment liquid tank 13. The treatment liquid tank 13 is provided with a connection port (not shown) for connecting the treatment liquid discharge pipe 14 and the treatment liquid return pump 15. The treatment liquid tank 13 and the head tank 19 are connected using the treatment liquid discharge pipe 14, the treatment liquid return pump 15, the cooler feed pipe 16, the cooler 17, and the treatment liquid return pipe 18 so that the liquid after the atomization treatment can be sent to the head tank 19. A discharge valve 24 and a discharge pipe 20 are connected to the head tank 19, and by opening and closing the discharge valve 24, the treatment liquid can be instantaneously returned to the raw material tank 2 at an arbitrary timing without requiring energy. Similar to the raw material supply pump 4, the treatment liquid return pump 15 is preferably a pump that can send the solid matter in the suspension without biting it and can send the liquid even when the viscosity increases. The cooler 17 is for reducing the temperature of the processing liquid, and it may be arranged between the outlet of the chamber 10 and the inlet of the raw material tank 2, or may be installed in the raw material circulation pipe 5. The installation position is not limited. The raw material temperature can also be controlled by adjusting the temperature and flow rate of the cold water sent to the cooler 17. Also, by using warm water instead of this cooling water or adding a heating device, the atomization treatment in the heating state can also be performed. Also, the outlet of the chamber outlet pipe 12 may not be connected to the inlet of the cooler 17, and the processing liquid tank 13, the processing liquid discharge pipe 14, the processing liquid return pump 15, and the cooler feed pipe 16 may not be provided. Furthermore, the processing liquid return pipe 18 may be connected to the outlet of the chamber 10 and directly returned to the raw material tank 2.

[0026] The raw material in a high-pressure state by the booster 8 is fed from the chamber supply ultra-high pressure pipe 9 to the high-pressure injection nozzle 11. The fed raw material is injected from the high-pressure injection nozzle 11 at a high pressure of 30 to 250 MPa to form an injection flow. The homogenization or atomization treatment of the raw material is performed by cavitation, collision of injection flows, collision with a hard object, etc. that occur when this injection flow is instantaneously and rapidly brought to a low-pressure state all at once. Note that as the high-pressure injection nozzle 11, a known high-pressure injection nozzle made of ceramics, diamond, sapphire, etc. that can inject a high-pressure fluid can be used. Here, the atomization treatment of the raw material may be performed multiple times on the solid matter in the raw material. That is, after the processing liquid obtained in the chamber 10 is sent to the raw material tank 2 using the processing liquid discharge pipe 14 or the like, the atomization treatment may be performed again in the chamber 10. The one subjected to the second atomization treatment is called 2pass.

[0027] When a plurality of high-pressure injection nozzles 11 connected to the chamber 10 are used and the injection flows are made to collide at an angle of the collision angle θ, the atomization progresses more easily. When there are two nozzles, the angle θ is preferably 95 to 178°, particularly preferably 100 to 170°. When it is less than 95°, for example, when the collision is at a right angle of 90°, structurally, there is a high possibility that the collision dispersion liquid directly collides with the wall portion of the chamber, and in many cases, the degree of polymerization decreases by more than 10% even with one-time atomization. On the other hand, when it is greater than 178°, for example, when the collision is 180°, that is, when the collision is head-on, the atomization effect is enhanced, but there is a possibility of damaging the opposing nozzle and peripheral equipment. When there are three nozzles, by setting the angle θ to 120°, it is possible to suppress the damage to the nozzles and peripheral equipment and maximize the collision efficiency.

[0028] Also, the number of times of the atomization treatment when performing the atomization treatment multiple times can be arbitrarily adjusted generally in the range of 2 to 200 times. When using a slurry liquid containing a raw material of long fibers as the raw material, the properties of the obtained treatment liquid become smoother and more homogeneous as the treatment is repeated, the solids in the liquid become finer, the fibers in the liquid become thinner and shorter. Therefore, it is possible to perform the atomization treatment with the number of repetitions according to the application.

[0029] The booster 8, which is a crank drive type, will be described using the structural diagram of FIG. 2. Note that FIG. 2 shows the booster having three plungers, and the number of plungers may be one, two, or four or more according to the treatment purpose and installation location. Also, for the purpose of suppressing pulsation, the number of plungers is preferably three or more. The booster 8 includes a crank portion 81 and a pump head 82.

[0030] The crank portion 81 includes a crankshaft 83 and power 35. The crankshaft 83 is composed of a crankshaft 30 and crank pins 31a, 31b, 31c arranged with a phase shift of about 120 degrees in the rotation direction. Power 35 is connected to journal 36, and main gear 33 is fitted to journal 36. Also, meshing gear 32 and crank journal 34 are fitted together, and meshing gear 32 and main gear 33 are arranged to mesh with each other. By doing so, the driving force of power 35 can rotate crankshaft 83. Power 35 can be an inverter motor. By doing so, the rotational speed of the crankshaft can be easily changed, and the discharge amount required for the miniaturization process can be controlled.

[0031] Crankshaft 83 is connected to connecting rods 29a, 29b, 29c via connecting rod connection shafts (not shown) respectively connected to crank pins 31a, 31b, 31c. Also, plungers 27a, 27b, 27c are coupled to connecting rods 29a, 29b, 29c by connecting pins 28a, 28b, 28c.

[0032] When crankshaft 83 rotates in the direction of arrow R, due to the oscillation of connecting rods 29a, 29b, 29c, plungers 27a, 27b, 27c reciprocate in the direction of arrow S. Here, since the reciprocating speed of the plunger at this time is determined by the gear ratio of meshing gear 32 and main gear 33, by appropriately setting these combinations, or by changing the rotational speed of power 35, the reciprocating speed of the plunger can be set to any range. The reciprocating speed of the plunger can be appropriately set according to the discharge pressure values of various positive displacement pumps. In the present invention, it is preferable to set the reciprocating speed of the plunger to 60 times / minute or more. Considering production efficiency, 100 times / minute or more is better, and 200 times / minute or more is even better. To suppress pulsation and make the equipment more stable, 300 times / minute or more is even better. Also, when it exceeds 1,000 times / minute, it is necessary to increase the supply pressure beyond the capacity of general-purpose pumps, so it is not preferable, 1,000 times / minute or less is preferable, and 800 times / minute or less is even more preferable.

[0033] By eccentrically connecting the connecting rods 29a, 29b, and 29c to the crank pins 31a, 31b, and 31c respectively, the timing of pressurized discharge of the suspension fluid can be shifted, the discharge pressure can be stabilized, and the efficiency of the atomization process can be improved. Therefore, the movement of the plunger will draw a sine curve, and the pulsation of the discharge pressure of the booster can be suppressed. Also, the movement with an accurate phase difference can be controlled, and the overlap of the sine curves can be reproduced.

[0034] The pump head 82 connected to the upper part of the crank portion 81 is provided with a communication port 25 for supplying the suspension fluid from the raw material tank 2 into the pump head 82 using the raw material supply pump 4. Also, separately from the communication port 25, it is provided with a connection port (not shown) for discharging the suspension fluid and returning the suspension fluid to the raw material tank 2. The raw material return pipe 7 is connected to the connection port. A high-pressure suspension fluid is supplied from inside the pump head 82 to the chamber supply ultra-high pressure pipe 9.

[0035] The pump head 82 will be described with reference to the structural diagram of FIG. 3. The pump head 82 connected to the upper part of the crank portion 81 includes a pressure chamber 37, a high-pressure side check valve 45 composed of a valve seat 39, a spring 38, and a ball 40, a low-pressure side check valve 46 composed of a valve seat 43, a spring 44, and a ball 42, a suction chamber 41, a raw material supply low-pressure flow path 47, and a raw material discharge high-pressure flow path 48. The low-pressure side check valve 46 and the piston seal assembly 26 are connected, and a space filled with the supplied suspension fluid is formed therebetween. The chamber supply ultra-high pressure pipe 9 is connected to the pressure chamber 37.

[0036] The flow of the raw material inside the pump head 82 is shown in Fig. 3 and is specifically shown below in the vertical relationship in the figure. The piston seal assembly 26 in which the plunger 27 is housed is arranged in the sliding direction of the plunger 27. When the upward rise of the plunger 27 stops inside the piston seal assembly 26 and it begins to be pulled downward, the ball 40 drops due to the force of the spring and the pressure in the pressure chamber 37, closing the lower gap, the ball 42 drops and the lower gap opens, and as the plunger 27 descends due to the pushing pressure of the raw material supply pump 4, the suspension fluid is quickly sucked into the space part inside the piston seal assembly 26 from the suction chamber 41 through the raw material supply low-pressure flow path 47 (from Fig. 3(i) to (ii)). Subsequently, as the suspension fluid is sucked in through the raw material supply low-pressure flow path 47 and the plunger 27 descends to the bottom inside the piston seal assembly 26 and starts to rise, the ball 42 rises due to the force of the spring and the pressure inside the piston seal assembly 26, closing the upper gap. Next, when the pressure rises to the discharge pressure and becomes higher than the pressure chamber 37, the ball 40 rises and the upper gap opens, and the suspension fluid is discharged into the pressure chamber 37 through the raw material discharge high-pressure flow path 48 (from Fig. 3(ii) to (iii)). The pressurized and discharged suspension fluid is sent under high pressure to the high-pressure injection nozzle 11 through the chamber supply ultra-high-pressure pipe 9.

[0037] The miniaturization processing apparatus according to the present invention having the above configuration has the following advantages. Hereinafter, as a specific example, the case where pulp containing long fibers is used as the raw material will be described. By circulating the suspension containing pulp between the two paths of the path of the raw material tank 2, the raw material discharge pipe 3, the raw material circulation pipe 5 and the raw material tank 2, and the path of the raw material discharge pipe 3, the raw material suction pipe 6, the booster 8 and the raw material return pipe 7, the pulp can be maintained in a state of flowing in the raw material circulation path. By setting such a state, it is possible to prevent the pulp mixture from staying and settling in the same path and the pulp concentration from rising, and to eliminate the malfunction at the initial stage of manufacturing start and the malfunction during manufacturing.

[0038] In addition, in the process of returning the treatment liquid discharged from the chamber 10 to the raw material tank 2 and performing the micronization treatment multiple times, even if the viscosity gradually increases due to the micronization of the pulp, by maintaining a flow rate of the raw material at a certain level or higher in the above two paths and circulating it, the thixotropic property of the raw material itself keeps the liquid in a low-viscosity flowing state, making it possible to stably perform the fiber micronization treatment.

[0039] Hereinafter, the present invention will be described based on examples, but the present invention is not limited to these examples. Also, the particle size distribution measurements described in the examples and comparative examples were measured by the following measurement methods.

[0040] (Measurement of particle size distribution) For the dispersion liquid after the micronization treatment, the particle size distribution was measured by the following measurement method. Each sample was put into a 50 ml centrifuge tube and pure water was added to prepare 40 g of a 0.1% finely divided cellulose fiber dispersion liquid. Then, the tip of a homogenizer (Ultra Turrax T18 manufactured by IKA) was inserted near the 25 ml scale of the centrifuge tube, and it was stirred at 10,000 rpm for 3 minutes for measurement. As the particle size distribution measuring device, Mastersizer 3000 (manufactured by Malvern Panalytical) was used. After the background measurement with the stirring speed of the particle size distribution measuring device set to 3,000 rpm, the sample was introduced. After the sample was introduced, the sample was measured 30 seconds later. After 5 measurements were completed, the device was washed, and the next sample was measured in the same procedure. The measurement results were adopted as the average value of 5 times of the "volume distribution" data.

[0041] (Example 1) Using the miniaturization processing apparatus according to the present invention described in FIG. 1, the discharge pressure of the raw material supply pump was set to 0.35 MPa, and miniaturization processing was performed using bamboo pulp with a solid concentration of 2% as the raw material at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / minute under inverter control. At that time, the pressure fluctuation of the pressure gauge arranged on the chamber inlet side was measured. Repeating the miniaturization process is called "pass", and repeating it X times is called "X pass". The measurement results of the pressure fluctuation within one minute of the measurement time are shown in FIG. 4.

[0042] (Comparative Example 1) In the wet pulverizer described in FIG. 6, the booster 110 was changed to a hydraulic booster type ultra-high pressure pump, and miniaturization processing was performed using softwood pulp with a solid concentration of 2% as the raw material at a pressure of 180 MPa. At that time, the pressure fluctuation of the pressure gauge arranged on the chamber inlet side was measured. The measurement results of the pressure fluctuation within one minute of the measurement time are shown in FIG. 5. The reciprocating speed of the plunger was 10 - 25 times / minute.

[0043] According to the graph shown in FIG. 4, the average injection pressure in Example 1 was 200.19 MPa, the standard deviation was ±2.39 MPa, the pressure range was about 15 MPa, and the pressure fluctuation range was about 8%. Also, according to the graph shown in FIG. 5, the average injection pressure in Comparative Example 1 was 176.11 MPa, the standard deviation was ±7.51 MPa, the pressure range was about 30 MPa, and the pressure fluctuation range was about 17%. It is considered that when the pressure fluctuation range is large, the risk of damage to equipment such as each pedestal, each pipe, the chamber, and the high-speed injection nozzle is high. Furthermore, as a secondary effect, in Example 1, the power unit required for 1 pass could be reduced by 37% compared to Comparative Example 1.

[0044] (Example 2) Using the miniaturization processing apparatus according to the present invention described in FIG. 1, the discharge pressure of the raw material supply pump was set to 0.35 MPa, and the miniaturization treatment using bamboo pulp with a solid concentration of 1.20% as the raw material was carried out at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / minute for 25 passes. For the dispersion liquid at the 20 - pass and 25 - pass time points in such miniaturization treatment, particle size distribution measurement was performed, and the volume - based average diameter and specific surface area were measured. The results are shown in Table 1 along with the time required for the miniaturization treatment.

[0045] (Example 3) Using the miniaturization processing apparatus used in Example 2, the discharge pressure of the raw material supply pump was set to 0.75 MPa, and the miniaturization treatment using bamboo pulp with a solid concentration of 1.25% as the raw material was carried out at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / minute for 35 passes. For the dispersion liquid at the 20 - pass, 25 - pass, and 35 - pass time points in such miniaturization treatment, particle size distribution measurement was performed, and the volume - based average diameter and specific surface area were measured. The results are shown in Table 1 along with the time required for the miniaturization treatment. Also, since the treatment liquid becomes smoother as the number of repetitions increases, it was confirmed that operation can be carried out without problems even when the discharge pressure of the raw material supply pump is lowered, and it can be operated even at 0.30 MPa.

[0046] (Example 4) Using the miniaturization processing apparatus used in Example 2, the discharge pressure of the raw material supply pump was set to 0.54 MPa, and the miniaturization treatment using bamboo pulp with a solid concentration of 1.19% as the raw material was carried out at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / minute for 25 passes. For the dispersion liquid at the 23 - pass and 25 - pass time points in such miniaturization treatment, particle size distribution measurement was performed, and the volume - based average diameter and specific surface area were measured. The results are shown in Table 1 along with the time required for the miniaturization treatment.

[0047] (Comparative Example 2) Using the wet grinding apparatus used in Comparative Example 1, a refining treatment was performed on bamboo pulp with a solid concentration of 1.19% as a raw material at a pressure of 200 MPa for 50 passes. For the dispersion liquid at the 50-pass point in such a refining treatment, a particle size distribution measurement was performed, and the volume-based average diameter and specific surface area were measured. The results are shown in Table 1 together with the treatment time required for 1 L of the refining treatment. The reciprocating speed of the plunger was 15 - 25 min -1 It was.

[0048]

Table 1

[0049] From the results of Comparative Example 2 in Table 1, in the wet grinding apparatus using a hydraulic booster type ultra-high pressure pump, in order to make the volume-based arithmetic average diameter 2.5 μm or less, 50 times of necessary repeated treatment times were required. On the other hand, when using the refining treatment apparatus according to the present invention, compared with the wet grinding apparatus using a hydraulic booster type ultra-high pressure pump, the number of refining treatment times is approximately half, and the volume-based arithmetic average diameter becomes 1.5 μm. From this result, it became clear that the time required for the refining treatment apparatus according to the present invention can be reduced to less than half. Also, considering the result that the power unit required for 1 pass could be reduced by 37% and suppressed to 63%, it became clear that the power could be significantly reduced to 31.5% (63% × 0.5) up to 68.5%. Also, since the pressure fluctuation range can be suppressed, it is considered that the reproducibility of the refining treatment is improved.

[0050] In the hydraulic booster type ultra-high pressure pump system, the piston reciprocating speed is slow, and it is considered to be in the boundary lubrication state in the Stribeck curve or near the boundary between the boundary lubrication state and the mixed lubrication state. Therefore, due to the increase in the load during piston sliding, the power unit required for 1 pass has become a large value. In this regard, it is considered that the supercharger in the crankshaft system has a high plunger reciprocating speed, and the plunger slides in the fluid lubrication zone of the Stribeck curve. Therefore, it is possible to reduce the size of the motor required for driving, and as a result, it is also possible to reduce the size of the miniaturization processing device itself.

[0051] (Example 5) In the miniaturization process of Example 4, the transmittance of the processing liquid obtained in each process from 1 pass to 25 passes was measured using an ultraviolet-visible spectrophotometer (manufactured by Hitachi High-Technologies Corporation: U-3900). A graph showing the plotted values is shown in FIG. 5.

[0052] (Comparative Example 3) In the miniaturization process of Comparative Example 2, the transmittance of the processing liquid obtained in each process from 1 pass to 50 passes was measured using an ultraviolet-visible spectrophotometer (manufactured by Hitachi High-Technologies Corporation: U-3900). A graph showing the plotted values is shown in FIG. 5.

[0053] From the graph in FIG. 7, it is considered that the transmittance in each pass is higher in Example 4, and even at the same number of processing times, the miniaturization process using the miniaturization processing device according to the present invention can perform a finer miniaturization process.

Explanation of Signs

[0054] 1: Micronization processing device, 2: Raw material tank, 3: Raw material discharge pipe, 4: Raw material supply pump, 5: Raw material circulation pipe, 6: Raw material suction pipe, 7: Raw material return pipe, 8: Booster, 9: Chamber supply ultra-high pressure pipe, 10: Chamber, 11: High-pressure injection nozzle, 12: Chamber outlet pipe, 13: Treatment liquid tank, 14: Treatment liquid discharge pipe, 15: Treatment liquid return pump, 16: Cooler feed pipe, 17: Cooler, 18: Treatment liquid return pipe, 19: Head tank, 20: Discharge pipe, 21: Product recovery pipe, 22: Product tank, 23: Stirring device, 24: Discharge valve, 25: Communication port, 26: Piston seal assembly, 27: Plunger, 28: Connecting pin, 29: Connecting rod, 30: Crankshaft, 31: Crank pin, 32: Meshing gear, 33: Main gear, 34: Crank journal, 35: Power, 36: Journal, 37: Pressure chamber, 38: Spring, 39: Valve seat, 40: Ball, 41: Suction chamber, 42: Ball, 43: Valve seat, 44: Spring, 45: High-pressure side check valve, 46: Low-pressure side check valve, 47: Raw material supply low-pressure flow path, 48: Raw material discharge high-pressure flow path, 81: Crank part, 82: Pump head, 83: Crankshaft, 107: Chamber, 108: High-pressure injection nozzle, 109: Tank, 110: Booster, 111: Heat exchanger

Claims

1. At least a raw material tank, a raw material supply pump, a raw material discharge pipe, a raw material suction pipe, a raw material return pipe and / or a raw material circulation pipe, a booster pump with a crank drive method and a plunger reciprocating speed of 60 - 1000 times / minute, a chamber equipped with a micronization processing means, a micronization processing device equipped with a processing liquid return pipe, the raw material supply pump and the raw material suction pipe are connected such that the raw material supply pump, the raw material tank and the raw material discharge pipe are connected, the raw material supply pump and the raw material suction pipe are connected, and the raw material suction pipe and the booster pump are connected, in order to pressurize and supply the raw material to the booster pump, the raw material circulation pipe and the raw material return pipe are connected in order to circulate the raw material between the booster pump and the raw material tank, the processing liquid return pipe is for returning the micronized processing liquid from the chamber to the raw material tank, a micronization processing device.

2. The raw material supply pump pressurizes and supplies the raw material to the booster pump at 0.2 MPa or more and 10 MPa or less, The micronization processing device according to Claim 1.

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