Micronization treatment 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 parts, chemical materials, food, medicine, 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 for miniaturizing 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 perspective 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 capable of slowly moving the plunger, and when the raw material liquid does not contain solid matter, since it is not necessary to use a hydraulic device capable of slowly operating the plunger, 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 round-trip speed of several seconds. For continuous micronization treatment 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 was discharged alternately from each hydraulic booster type ultra-high pressure pump at intervals of several seconds, 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. This pressure fluctuation caused problems such as damage inside the ultra-high pressure components due to wear and tear and breakage due to deterioration, and wear of the seal components of the cylinder head sliding at a low speed. Also, generally, since the hydraulic booster type ultra-high pressure pump is large, the entire micronization treatment apparatus including this pump becomes large, requiring a large installation area and resulting in high introduction costs.

[0006] On the other hand, in the case of a suspension fluid with high viscosity or a slurry fluid containing solids, fibers, or powders, if a crank type plunger pump is adopted, since the plunger drive 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 under negative pressure.

[0007] Therefore, in view of the above problems, the present invention provides a micronization treatment apparatus that is capable of micronizing a suspension fluid with high viscosity or a slurry fluid containing solids, fibers, or powders (hereinafter sometimes referred to as a suspension fluid), and can suppress equipment damage and the like caused by 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, and further to stabilize the pressure fluctuation range of the high-pressure suspended fluid discharged, and to perform a reliable micronization process using a stable ultra-high pressure flow, thereby reducing the number of micronization processes and providing 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 have found that even when performing a micronization process on a suspension, the driving method of the pressure booster is a crankshaft method with a high plunger reciprocating speed, and the movement of the plunger is made regular and periodic at high speed, and by increasing the discharge pressure of the raw material supply pump to stably supply the suspended fluid to the pressure booster, it is possible to suppress the fluid pressure fluctuation of the suspended fluid and increase the amount of micronization process 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 pressure 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 pressure 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.

Effect of the Invention

[0011] According to the micronization processing apparatus of the present invention, there is provided a micronization processing apparatus capable of micronizing 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 suspended 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 miniaturization processing apparatus according to the present invention will be described in detail. However, the following embodiments are for assisting in understanding 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 the miniaturization processing, and is used for a slurry liquid having a high viscosity containing such a raw material, or a slurry liquid containing solid components, fibers, or powders. The term "miniaturization processing" in this specification means subjecting the raw material in a high-pressure state using a booster to some physical treatment. The "processing liquid" in this specification refers to the liquid after the miniaturization processing is performed on the raw material. In other words, it refers to the raw material liquid that has passed through the miniaturization processing apparatus one or more times.

[0015] As shown in FIG. 1, the miniaturization processing apparatus 1 of the present 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 the 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 the raw material tank 2 via the raw material discharge pipe 3.

[0017] Examples of the raw materials include starch powder, polyvinyl alcohol powder, dissolved cellulose powder, etc. which have poor solubility and tend to form lumps, and become highly viscous solutions, as well as polysaccharide-derived cellulose fibers containing natural plants such as wood fibers, bamboo fibers, sugarcane fibers, seed hair fibers, leaf fibers, etc. that require refinement, or those obtained by chemically modifying these. As other raw materials, those used in the chemical industry, such as dispersion of toner, preparation of aqueous paints, wet dispersion and crushing of organic and inorganic powders and colored pigment powders, etc., and those used in the electronic component industry, such as wet dispersion and crushing of organic and inorganic powders, etc., can be appropriately used 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 process described later, those obtained by chemically modifying raw materials such as pulp can also be used as raw materials in the present embodiment. Examples include hydrolysis of polysaccharides by acids, hydrolysis of polysaccharides by enzymes, swelling of polysaccharides by alkalis, oxidation of polysaccharides by oxidants, reduction of polysaccharides by reducing agents, oxidation by TEMPO catalysts, phosphoric esterification, carbamation, cationization, etc.

[0019] The raw material supply pump 4 is preferably a pump that can send without biting into the solids in the suspension and can send the liquid even when the viscosity increases, and a positive displacement metering pump is preferred. Among positive displacement metering pumps, non-contact pumps are preferred from the viewpoint of preventing foreign substances such as contaminant powder from clogging the injection nozzle, and particularly, 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 is possible to prevent poor suction of the raw material liquid.

[0020] In addition, to the raw material supply pump 4, a raw material suction pipe 6, a raw material circulation pipe 5, and a pressure regulating valve (not shown) are connected. Furthermore, a switching valve (not shown) or the like may be provided in the raw material circulation pipe 5 and the raw material suction pipe 6 so that the liquid can be sent to either one of them. By connecting in this way, it is possible to circulate the suspension fluid between the pressurizer 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 using only the raw material return pipe 7 without using the raw material circulation pipe 5. By doing so, the locations 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 pressurizer can be made constant, and the operability of the miniaturization treatment apparatus according to the present invention is stabilized. Also, 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 wears, the valve opening degree tends to decrease.

[0022] To the raw material circulation pipe 5, a product recovery pipe 21 for recovering the product after performing the miniaturization treatment a specified number of times is connected, and to the product recovery tank 21, a product tank 22 is connected. 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, and in that case, the product can be obtained at a high temperature.

[0023] The chamber 10 is provided with a miniaturization treatment means for performing the miniaturization treatment inside the chamber. Examples of the miniaturization treatment means include means for performing the 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, a case where a high-pressure injection nozzle is used for the miniaturization treatment as the miniaturization 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 raw material is miniaturized in the chamber 10. Further, the chamber 10 can be connected with a chamber outlet pipe 12, a treatment liquid tank 13, a treatment liquid discharge pipe 14, a treatment liquid return pump 15, a cooler feed pipe 16, a cooler 17, and a treatment liquid return pipe 18 according to the number of miniaturization 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. Also, 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 miniaturization treatment efficiency can be enhanced.

[0025] The chamber outlet pipe 12 is used to take out the liquid after the raw material has been miniaturized 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 miniaturization 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. By opening and closing the discharge valve 24, the treatment liquid can be returned to the raw material tank 2 instantaneously 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 by adding a heating device, the atomization treatment in the heated 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. Further, 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. By suddenly reducing the pressure of this injection flow to a low-pressure state all at once, cavitation, collision between injection flows, collision with a hard object, etc. occur, and the homogenization or atomization treatment of the raw material is performed. 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 jets are made to collide at an angle of the collision angle θ, the refinement 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 in a right-angled state of 90°, there is likely to be a portion where the collision dispersion liquid directly collides with the wall portion of the chamber structurally, and in many cases, the degree of polymerization decreases by more than 10% even with one-time refinement. On the other hand, when it is greater than 178°, for example, when the collision is 180°, that is, when the collision is made face-to-face, the refinement effect is enhanced, but there is a case where the opposing nozzle and peripheral equipment may be damaged. 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 while maximizing the collision efficiency.

[0028] Also, as the number of times of refinement processing when performing multiple refinement processes, it can be arbitrarily adjusted generally in the range of 2 to 200 times. When using a slurry liquid containing a long fiber raw material 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 refinement processing with the number of repetitions according to the application.

[0029] The booster 8, which is a crank drive system, will be described using the structural diagram of Fig. 2. Note that Fig. 2 shows the booster when it has 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 crankshaft 83 can be rotated by the driving force of power 35. The power 35 can be an inverter motor. By doing this, the rotational speed of the crankshaft can be easily changed, and the discharge volume required for the miniaturization process can be controlled.

[0031] The crankshaft 83 is connected to connecting rods 29a, 29b, 29c via connecting rod connecting 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 coupling pins 28a, 28b, 28c.

[0032] When the 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 made within an arbitrary range. The reciprocating speed of the plunger can be appropriately set according to the discharge pressure values of various volumetric metering 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. For suppressing pulsation and making 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 a general-purpose pump, 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 pressure 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, a connection port (not shown) for discharging the suspension fluid and returning the suspension fluid to the raw material tank 2 is provided. 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 is provided with 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 within the pump head 82 is shown in Fig. 3 and is specifically described below in terms of 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 movement of the plunger 27 stops within the piston seal assembly 26 and it begins to be pulled downward, the ball 40 descends due to the force of the spring and the pressure in the pressure chamber 37, closing the lower clearance, the ball 42 descends opening the lower clearance, and the suspension fluid is quickly inhaled from the suction chamber 41 through the raw material supply low-pressure flow path 47 into the space portion within the piston seal assembly 26 as the plunger 27 descends due to the pushing pressure of the raw material supply pump 4 (from Fig. 3(i) to (ii)). Subsequently, as the suspension fluid is inhaled through the raw material supply low-pressure flow path 47 and the plunger 27 descends to the bottom within the piston seal assembly 26 and then starts to rise, the ball 42 rises due to the force of the spring and the pressure within the piston seal assembly 26, closing the upper clearance. Then, when the pressure rises to the discharge pressure and becomes higher than that in the pressure chamber 37, the ball 40 rises opening the upper clearance, 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 at high pressure to the high-pressure injection nozzle 11 through the chamber supply ultra-high-pressure piping 9.

[0037] The micronization 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 within the raw material circulation path. By setting such a state, it is possible to prevent the pulp mixture from staying and settling within the same path and the pulp concentration from increasing, and to eliminate the malfunction at the initial stage of manufacturing start and the malfunction during manufacturing.

[0038] Also, in the process of returning the treatment liquid discharged from the chamber 10 to the raw material tank 2 and performing the fibrillation treatment multiple times, even if the viscosity gradually increases due to the fibrillation of the pulp, by always maintaining a flow rate of the raw material at a certain level or higher and circulating it through the above two paths, the thixotropic property of the raw material itself keeps the liquid in a low-viscosity flowing state, enabling the stable implementation of the fiber fibrillation 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] (Particle size distribution measurement) The particle size distribution of the dispersion after the fibrillation treatment was measured by the following measurement method. Each sample was placed in a 50 ml centrifuge tube, pure water was added, and 40 g of a 0.1% finely divided cellulose fiber dispersion was prepared. Next, the tip of a homogenizer (Ultra-Turrax T18 manufactured by IKA) was inserted near the 25 ml mark of the centrifuge tube, and the mixture was stirred at 10,000 rpm for 3 minutes for measurement. The particle size distribution measuring device used was Mastersizer 3000 (manufactured by Malvern Panalytical). After background measurement with the stirring speed of the particle size distribution measuring device set at 3,000 rpm, the sample was introduced. The sample was measured 30 seconds after the sample was introduced. 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 data of "volume distribution".

[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 the miniaturization processing using bamboo pulp with a solid concentration of 2% as the raw material was carried out at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / minute by inverter control. At that time, the pressure fluctuation in the pressure gauge arranged on the chamber inlet side was measured. Incidentally, repeating the miniaturization process is called "pass", and repeating it X times is called "X pass". The pressure fluctuation measurement results for one minute within 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 the miniaturization process using softwood pulp with a solid concentration of 2% as the raw material was carried out at a pressure of 180 MPa. At that time, the pressure fluctuation in the pressure gauge arranged on the chamber inlet side was measured. The pressure fluctuation measurement results for one minute within the measurement time are shown in FIG. 5. Incidentally, 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 in a state where the pressure fluctuation range is large, the risk of damage to facilities 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 micronization processing apparatus according to the present invention shown in FIG. 1, the discharge pressure of the raw material supply pump was set to 0.35 MPa, and micronization processing was performed with bamboo pulp having a solid concentration of 1.20% as the raw material at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / min for 25 passes. Regarding the dispersion liquid at the 20 - pass and 25 - pass points in such micronization processing, particle size distribution measurement was performed, and the volume - based average diameter and specific surface area were measured. Along with the time required for the micronization processing, the results are shown in Table 1.

[0045] (Example 3) Using the micronization processing apparatus used in Example 2, the discharge pressure of the raw material supply pump was set to 0.75 MPa, and micronization processing was performed with bamboo pulp having a solid concentration of 1.25% as the raw material at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / min for 35 passes. Regarding the dispersion liquid at the 20 - pass, 25 - pass, and 35 - pass points in such micronization processing, particle size distribution measurement was performed, and the volume - based average diameter and specific surface area were measured. Along with the time required for the micronization processing, the results are shown in Table 1. Also, since the processing 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 micronization processing apparatus used in Example 2, the discharge pressure of the raw material supply pump was set to 0.54 MPa, and micronization processing was performed with bamboo pulp having a solid concentration of 1.19% as the raw material at a pressure of 200 MPa and a plunger reciprocating speed of 400 - 500 times / min for 25 passes. Regarding the dispersion liquid at the 23 - pass and 25 - pass points in such micronization processing, particle size distribution measurement was performed, and the volume - based average diameter and specific surface area were measured. Along with the time required for the micronization processing, the results are shown in Table 1.

[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 at the 50 - pass point in such a refining treatment, the particle size distribution was measured, and the volume - based average diameter and the specific surface area were measured. The results are shown in Table 1 together with the treatment time per liter required for the refining treatment. Note that 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 repeated treatment 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 was approximately half, and the volume - based arithmetic average diameter became 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 per pass was reduced by 37% and suppressed to 63%, it became clear that the power can be significantly reduced by 68.5% to 31.5% (63%×0.5). Also, since the pressure fluctuation range can be suppressed, it is considered that the reproducibility of the refining treatment becomes high

[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 per pass has become a large value In this regard, it is considered that in the supercharger using the crankshaft method, the reciprocating speed of the plunger is high, and the sliding of the plunger is carried out in the fluid lubrication zone in the Stribeck curve. Therefore, it is possible to reduce the size of the motor required for driving, and as a result, it is 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 plotting each value 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 plotting each value 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 be performed more finely and minutely.

Explanation of Signs

[0054] 1: Micromachining 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: Delivery 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: Crank shaft, 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 system, and a chamber equipped with a miniaturization processing means, a miniaturization processing apparatus comprising: the raw material supply pump and the raw material suction pipe are for pressurizing and supplying the raw material to the booster pump, the raw material circulation pipe and the raw material return pipe are for returning the raw material to the raw material tank, a miniaturization processing apparatus.

2. 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 plunger reciprocating speed of 60 times / minute or more, and a chamber equipped with a miniaturization processing means, a miniaturization processing apparatus comprising: the raw material supply pump and the raw material suction pipe are for pressurizing and supplying the raw material to the booster pump, the raw material circulation pipe and the raw material return pipe are for returning the raw material to the raw material tank, a miniaturization processing apparatus.

3. 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 system, a chamber equipped with a miniaturization processing means, and a processing liquid return pipe, a miniaturization processing apparatus comprising: the raw material supply pump and the raw material suction pipe are for pressurizing and supplying the raw material to the booster pump, the raw material circulation pipe and the raw material return pipe are for returning the raw material to the raw material tank, the processing liquid return pipe is for returning the processed processing liquid to the raw material tank, a miniaturization processing apparatus.

4. 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 plunger reciprocating speed of 60 times / minute or more, a chamber equipped with a miniaturization processing means, and a processing liquid return pipe, a miniaturization processing apparatus comprising: the raw material supply pump and the raw material suction pipe are for pressurizing and supplying the raw material to the booster pump, the raw material circulation pipe and the raw material return pipe are for returning the raw material to the raw material tank, the processing liquid return pipe is for returning the processed processing liquid to the raw material tank, a miniaturization processing apparatus.

5. 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 miniaturization processing apparatus according to any one of claims 1 to 4.

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