CN101219352A - Emulsification device and microparticle manufacturing device - Google Patents

Abstract

The emulsification device and microparticle production device of the present invention can produce a large amount of particles with a controlled particle size. The microparticle manufacturing device (100) is equipped with a fluid device (114). The fluid device (114) has a fine flow path provided with a throttle plate (203-205) for forming a jet flow of the liquid, and a device for actively vibrating the liquid. The flow path wall of the piezoelectric element (206, 207), and the device (111) used to measure the particle size and quantity of the particles floating in the fluid. The piezoelectric element vibrates sideways in the same direction as the flow direction of the fluid.

Description

Emulsification device and microparticle manufacturing device

technical field

The present invention relates to an apparatus for emulsifying a raw material or a microparticle manufacturing apparatus for micronizing a raw material to produce fine particles.

Background technique

A conventional emulsification device is described in Patent Document 1, for example. In the emulsion production method described in this gazette, in order to quickly and easily liquefy the aqueous emulsion of the rosin compound, the emulsifier aqueous solution is supplied to the orifice plate (Orifis) under high pressure from a high-pressure discharge emulsifier, and the molten The rosin-like compound is supplied to the high-speed ejection part from another flow path, and collides at a mixing temperature within a predetermined temperature range. Then, the mixture is introduced into the absorbing unit part in which the units are inserted in a multi-stage shape, and discharged from the emulsion discharge part.

An example of a stirring type emulsion production method widely used in the prior art is described in Patent Document 2. In the method for producing an agitated emulsion described in this gazette, 100 parts by weight of a high-viscosity liquid organopolysiloxane having a viscosity of 10,000 cSt to 1,000,000 cSt at 25° C. is put into 1 to 20 parts by weight of an ionic emulsifier aqueous solution. Stir and disperse in the weight section. Then, 1 to 50 parts by weight of a nonionic emulsifier is charged, and the particle size is reduced by high-speed shear stirring (high shear stirring する), and finally diluted with water.

Furthermore, Patent Document 3 describes another method for producing an emulsion. In this publication, in order to generate a high-quality emulsion with a uniform particle size in a mass-producible manner, the microemulsifier has a plurality of inlets and one outlet, and a plurality of channels formed in multiple stages between these inlets and outlets, The channel is used to sequentially mix the fluids respectively introduced from the inlets and then introduce them into the outlet. Moreover, the cross-sectional area of each stage of the flow path formed by each microchannel narrows sequentially from the inlet side to the outlet side, and the closer to the outlet side, the more the shear velocity and its dispersion effect can be increased.

Patent Document 1 Japanese Patent Application Laid-Open No. 2000-210546

Patent Document 2 Japanese Patent Application Laid-Open No. 7-173294

Patent Document 3 Japanese Patent Application Laid-Open No. 2004-81924

In the existing emulsion liquefaction equipment or emulsification equipment, there is a problem of how to apply the technology that has succeeded in small-scale laboratory-level production to industrial mass production. In the production of the aqueous emulsion described in the above-mentioned Patent Document 1, it is necessary to spray the solution at a high pressure of 250 MPa under high pressure, and preparing such high-pressure equipment in the actual production equipment will result in a huge device and increase the cost. Moreover, solutions that cannot withstand high pressure cannot be used, and the types of solutions are limited.

In the method for producing an emulsion described in Patent Document 2, the high-viscosity first solution is poured into the second aqueous solution and stirred, and then high-speed shear stirring is performed under the third emulsifier. However, in the method described in this gazette, what can be used is easily limited to a special solution, and emulsification of general oil and aqueous solution may not always be usable.

Furthermore, Patent Document 3 describes a technique for realizing an emulsion of immiscible fluids such as water and oil by microfabrication. This method can produce an emulsion with uniform particle size, but the diameter of the droplet is dominated by the flow rate of the liquid flow. Therefore, in order to obtain the desired droplet diameter, the flow rate of the liquid flow must sometimes be sacrificed. In this case, a large amount of processing If not, the size of the device will be increased or the processing time will be prolonged. As another method, there is a method of applying ultrasonic waves to utilize shock waves generated by cavitation in a liquid, but in this case, it is difficult to apply to raw materials containing biopolymer materials such as proteins that lose activity at high temperatures.

Contents of the invention

The present invention has been made in view of the above-mentioned problems of the prior art, and an object thereof is to facilitate the control of the properties of the emulsion in an emulsification device and to enable a large amount of emulsion to be generated. Another object of the present invention is to enable a microparticle manufacturing apparatus to produce a large amount of particles with a controlled particle size. And the object of the present invention is to achieve any one of these objects.

In order to achieve the above object, the feature of the present invention is that the device is equipped with a fluid device, and the fluid device has a fine flow path for forming the liquid into a jet, and a flow path wall for actively vibrating the liquid; the flow path for actively vibrating The road wall vibrates sideways in the same direction as the liquid flow. Also in this feature, it is preferable that the flow path wall for active vibration has a piezoelectric element, and the surface of the piezoelectric element on the side contacting the liquid is coated with an insulating material.

In addition, in order to achieve the above-mentioned purpose, the device is equipped with a fluid device having a fine flow path for forming the liquid into a jet, a flow path wall for actively vibrating the liquid, and a device for measuring suspended particles in the fluid. Particle size and number means.

Furthermore, in this feature, it is preferable that the fine flow path is provided with multi-stage throttle plates that generate jet flow and vortex flow, and it is preferable that the flow path wall that actively vibrates is on the upper side in the same direction as the liquid flow direction. Slip vibration. In addition, it is also possible that the actively vibrating channel wall has a piezoelectric element, and the surface of the piezoelectric element in contact with the liquid is coated with an insulating material. Preferably, the device is an emulsification device or a particle production device. Furthermore, the device may connect a plurality of fluid devices in parallel.

According to the present invention, the raw materials to be emulsified (water raw materials and oily raw materials) are emulsified into emulsions at the level of tens to hundreds of microns by means of the high shear stress accompanying jet flow, and then the flow path walls are Actively vibrating and applying an appropriate shear stress to refine the particles to a desired particle size, so that the characteristics of the emulsion in the microparticle manufacturing device and emulsification device can be easily controlled. Moreover, according to the present invention, the flow paths that can generate jets and shear stresses of arbitrary intensity can be connected in parallel in the original state corresponding to the desired processing capacity, thereby avoiding the increase in scale based on the law of physical similarity in the prior art. However, there is a problem that a large amount of particles whose particle size is controlled in the fine particle manufacturing device and the emulsification device is generated.

Description of drawings

Fig. 1 is a block diagram of an embodiment of a microparticle manufacturing apparatus according to the present invention.

FIG. 2 is a diagram for explaining a channel structure of an emulsification facility having the microparticle manufacturing apparatus shown in FIG. 1 .

Fig. 3 is a diagram for explaining the outflow structure of the emulsification facility having the microparticle manufacturing apparatus shown in Fig. 1 .

Fig. 4 is a diagram for explaining generation of a complex emulsion.

Symbol Description

100, 100b particle manufacturing device (emulsification device)

203～205 Throttle plate

206, 207 Piezoelectric elements

208a, 208b flow path

208c combined flow path

208d emulsification flow path

208f Expansion Department

313 Passive emulsification department

314 Active emulsification department

Detailed ways

One embodiment of the emulsification device or particle production device according to the present invention will be described below with reference to the drawings. In FIG. 1 , a system of a microparticle manufacturing apparatus 100 is shown in a block diagram. The microparticle manufacturing apparatus 100 has a tank 101 for storing a raw material A (dispersed phase) to be emulsified, and a tank 102 for storing a raw material B (continuous phase) in which the raw material A is dispersed. The emulsification device 103 , which will be described in detail later, mixes these raw materials A and B to emulsify them.

The first pump 104 sends the liquid of the raw material A from the tank 101 to the emulsification device 103 through the pipe 107 . Similarly, the second pump 105 sends the liquid of the raw material B from the tank 102 to the emulsification device 103 through the pipe 108 . The emulsified mixture liquid of the raw material A and the raw material B is sent from the emulsification device 103 to the tank 106 through the piping 109 and collected.

A detour channel 110 is provided on the pipe 109 for the mixture. A particle size distribution meter 111 is provided on the bypass flow path 110 . The particle size distribution meter 111 can monitor the particle diameter of the dispersed phase in the mixture flowing out from the emulsification device 103 on-line. In the flow path of the emulsification device 103, a piezoelectric element capable of actively vibrating the flow path is provided. The piezoelectric element is driven by a piezoelectric element driving circuit 112 .

The first and second liquid delivery pumps 104 and 105 , the piezoelectric element drive circuit 112 and the particle size distribution meter 111 are connected to the user console 113 . The console 113 is used by a user of the microparticle manufacturing apparatus 100 to monitor the particle size distribution of the currently generated mixture. Moreover, the ratio of the delivery volume of the raw material A liquid and the raw material B liquid delivered by the first and second liquid delivery pumps 104, 105, the delivery volume, and the vibration intensity of the piezoelectric element in the emulsification device 103 are adjusted to generate the required mixture. The emulsification device 103 and the particle size distribution meter 111 constitute an emulsification unit 114 .

In FIG. 2 , the emulsification device 103 included in the microparticle manufacturing apparatus 100 shown in FIG. 1 is shown in a vertical cross-sectional view. The raw material liquids sent from the raw material tanks 101 and 102 by the liquid feeding pumps 104 and 105 respectively flow into the flow paths 208a and 208b in the emulsification device 103 as shown in 201 and 202, and merge in the combining flow path 208c. It then passes through the damper plates 203, 204, 205, passes through the enlarged portion 208f provided with the piezoelectric elements 206, 207 on the wall surface, and flows out to the outside of the device through the flow path 208d as shown in 209. The piezoelectric elements 206 and 207 can be externally controlled to vibrate in the thickness-slip vibration mode, as indicated by dotted lines in the figure.

If considering the connection between the emulsification device 103 and the piping, that is, the piping connection with the flow paths 208a, 208b as the inlets of the raw materials A and B, and the flow path 208d as the outlet of the emulsion dispersion, it is preferable to make these flow The cross section of the road is circular.

Between the joint flow path 208d and the enlarged portion 208f, three kinds of orifice plates 203-205 are spaced apart from each other and arranged sequentially in the flow direction of the liquid flow. The first throttle plate 203 is located on the most upstream side, and a hole is formed in the center, and its opening ratio is the largest among the three throttle plates 203 to 205 . The second throttle plate 204 arranged in the middle has a conical shape in which the center portion of the side surface on the upstream side is recessed toward the downstream side, and the downstream side is a surface perpendicular to the flow direction of the emulsification flow path 8d. Furthermore, the opening ratio of the opening formed in the central portion of the second throttle plate 204 is the smallest among the first to third throttle plates 203 to 205 .

In addition, when passing through the enlarged portion 208f where the piezoelectric element is provided on the wall surface, the flow velocity is reduced, thereby gaining time to pass through the portion (208f portion). Therefore, the cross-sectional area of the portion 208f may be set larger than that of other flow path portions.

In addition, it is preferable to generate as much vibrating shear stress as possible in the enlarged part 208f to uniformly generate particles. Therefore, even if the cross-sectional shape of the other flow path parts is circular, only this flow path part is preferably formed so that two A rectangular cross-sectional shape in which planar piezoelectric elements are arranged facing each other. Although the interval between two facing piezoelectric elements is also determined by the vibration frequency and the viscosity of the stock solution, generally making it as narrow as possible can produce the same vibration shear stress.

The figure shows the case where gaps are provided between the piezoelectric elements 207, 208 and the flow path walls on which these piezoelectric elements are provided, and the sideslip vibration shown by the dotted lines will not be hindered. If the undiluted solution remains and causes a problem in terms of sanitation, the gap may be sealed with a highly stretchable elastic material.

The behavior of the mixed fluid in the enlarged portion 208f in the emulsification device 103 shown in FIG. 2 will be described with reference to FIG. 3 . FIG. 3( a ) is a diagram for explaining the flow of the throttle plates 203 to 205 , and FIG. 3( b ) is a diagram for explaining the flow of the enlarged portion 208 f . As described above, the orifice diameter 307 of the second throttle plate 204 is set smaller than the orifice diameter 306 of the first throttle plate 203 .

Based on this, when the flow rate of the mixed flow of raw materials A and B exceeds a predetermined flow rate, a secondary flow 308 that is a vortex flow is formed in the flow path between the first throttle plate 203 and the second throttle plate 204 . Through the secondary flow 308, the dispersed phase (raw material A) 302 of the raw material flowing from the upstream side between the first and second throttle plates 203, 204 is mixed with the continuous phase (raw material B) 301, and dispersed into relatively large Droplet309.

Furthermore, since the orifice diameter 307 smaller than the orifice diameters of the first and third orifice plates 203 and 205 is formed in the second orifice plate 204 , the orifice is formed toward the downstream side of the second orifice plate 204 Intense Jet 310. Furthermore, the liquid droplets 309 formed between the first and second throttle plates 203 , 204 are split into fine liquid droplets 311 by the strong shear stress generated by the jet flow 310 .

The jet 310 generated towards the downstream side of the second throttle plate 204 gradually widens as it goes downstream. Therefore, in this state, the third orifice plate 205 whose opening is wider than the second orifice plate 204 cannot pass through, and part of the liquid flow returns to form the secondary flow 312 that flows backward toward the upstream side. The secondary flow 312 is further mixed with the fine dispersed phase (raw material A) and the continuous phase (raw material B), and flows downstream through the opening of the third throttle plate 305 .

As described above, the piezoelectric elements 206 and 207 are arranged facing each other on the enlarged portion 208f formed downstream of the first to third throttle plates 203 to 205 . The piezoelectric elements 206 and 207 generate side-slip vibration on the wall surface of the flow path, and split the droplets of the mixed liquid of raw material A and raw material B into finer pieces. Here, the piezoelectric elements 206 and 207 vibrate in phases opposite to each other as shown in FIG. 3( b ). In this way, an oscillating flow velocity distribution 315 , 316 is formed between the two piezoelectric elements 206 , 207 . The shear stress is generated by the flow velocity distribution 315, 316, and the shear stress forms the spherical liquid droplet flowing from the upstream into the elongated liquid droplet 317 stretched in the flow direction, and finally the elongated liquid droplet 317 is subdivided into a plurality of approximately spherical droplets. As a result, finer droplets are generated.

The distribution state of the vibration-type flow velocity distribution can be controlled by the vibration velocity 318 in the sideslip direction of the piezoelectric elements 206 and 207 . That is, the number of times the droplet is torn when the droplet 319 passes can be determined by the time between the droplet 319 passing through the piezoelectric elements 206 and 207 and the vibration frequency of the wall surface vibration. Therefore, the vibration number and the vibration displacement of the wall surface vibration are adjusted according to the shear stress required for the splitting of the raw materials A and B and the flow speed of the raw materials A and B. Thus, raw materials A and B can be emulsified into desired particle diameters.

Typically a high voltage is applied across the piezoelectric elements 206,207. Therefore, the surfaces of the piezoelectric elements 206, 207 connected to the materials A, B must be insulated. In this embodiment, although not shown in the drawing, an insulating and highly elastic resin is applied to the surfaces of the piezoelectric elements 206 and 207 .

In the following description, the first to third throttle plates 203 to 205 are referred to as a passive emulsification portion 313 , and the enlarged portion 208 f is referred to as an active emulsification portion 314 . In the above-described embodiment, the emulsification device 103 has both the passive emulsification unit 313 and the active emulsification unit 314 , the former 313 performs rough emulsification, and the latter 314 generates fine particles. Therefore, in the desired mixing state, the emulsification device 103 may have only any emulsification section.

In addition, in order to generate finer particles, the passive emulsification part 313 and the active emulsification part 314 may be provided in multiple stages as required. The combination of these emulsifying parts 313 and 314 corresponds to the physical properties such as the viscosity and density of the raw materials A and B to be emulsified, the interfacial tension between the raw materials A and B, and the average particle diameter and particle size distribution of the target particles. Mixed state to decide.

In FIG. 3( b ), the piezoelectric elements 206 and 207 are provided to face the enlarged portion 208f so that they vibrate in opposite phases, but only one piezoelectric element may be provided. Also in this case, the emulsification channel 208d preferably has substantially the same cross-sectional area in the flow direction. The strength of the generated shear stress is weaker than the case where the two piezoelectric elements 206 and 207 are arranged facing each other, but there is an advantage that the power consumed by the active emulsification part 314 can be reduced and only one drive circuit for driving the piezoelectric element is required. That's it. As long as the droplet passage time is prolonged corresponding to the portion where the shear stress is weakened, the same effect as that of the case where piezoelectric elements are arranged facing each other can be obtained, so it is particularly effective in processing with a relatively small amount of processing.

Another embodiment of the microparticle manufacturing apparatus according to the present invention is illustrated with FIG. 4 . In the above-mentioned embodiment, two kinds of raw materials A, B are mixed and emulsified, but in the present embodiment, more than three raw materials A, B, C, ... are emulsified to generate so-called composite emulsion (ダブルエママLucian). In FIG. 4 , three kinds of raw materials A, B, and C are used for easy understanding. When using three kinds of raw materials A, B, and C, only one emulsification facility 103b is added.

In Fig. 4(a), a microparticle manufacturing apparatus 100b for generating a complex emulsion is shown in block diagram form. In FIG. 4( a ), illustration of the user console and the connection lines with the user console is omitted. The emulsification unit 114b has two emulsification devices 103, 103b. A mixed solution 402 of raw material A (dispersed phase) and raw material B (continuous phase) is generated from the emulsification device 103 . The added emulsification device 103b introduces the raw material C into the mixed solution of the raw materials A and B to disperse it, and finally generates a composite emulsion 404 of A/B/C. In order to collect the complex emulsion, a tank 106 is provided downstream of the added emulsification device 103b.

FIG. 4( b ) schematically shows the mixed state of the respective raw materials AC in the emulsification unit 114 b in FIG. 4( a ). On the upstream side, raw material A is mixed with raw material B, and on the downstream side, raw material C is mixed into the mixed raw materials A, B. By repeating these steps in sequence, an emulsion of four or more raw materials can be produced. At this time, the diameter of the particles can be changed by the throttle plate, the electric power applied to the piezoelectric element, or the like.

According to each of the above-described embodiments, the particle size of the emulsion can be easily controlled, and moreover, multiple structures of the emulsion can be easily generated. In the case of mass-producing equipment from a laboratory level, blocks of emulsification units are connected in parallel to a plurality of columns. At the laboratory level, one or more emulsification units are used to generate the desired emulsion. When converting to mass production by equipment, the emulsification units are connected in parallel according to the processing capacity. Through the above steps, the problem of increasing scale based on the similarity law in the prior art can be avoided. The embodiments of the present invention have been described above, but the present invention is not limited to the above-described embodiments. The summary of the invention describes the true spirit of the invention.

Claims (8)

1. emulsifier unit or fine-grain manufacturing apparatus is characterized in that described device has carried fluid device, and this fluid device has the stream wall that is used for that liquid formed the fine channel of jet and is used for liquid is carried out active vibration; The vibration of on the direction identical, breakking away of the described stream wall that carries out active vibration with liquid flow direction.

2. emulsifier unit as claimed in claim 1 or fine-grain manufacturing apparatus is characterized in that, the described stream wall that carries out active vibration has piezoelectric element, described piezoelectric element in the surface-coated that contacts that side with liquid insulating materials.

3. fine-grain manufacturing apparatus, it is characterized in that, described device has carried fluid device, this fluid device have be used for liquid form jet fine channel, be used for carrying out the stream wall of active vibration and be used for measuring the particle diameter of particles suspended in the fluid and the device of quantity.

4. fine-grain manufacturing apparatus as claimed in claim 3 is characterized in that described fine channel is provided with the multi-level throttle plate, and described choke block produces jet and eddy current.

5. fine-grain manufacturing apparatus as claimed in claim 3 is characterized in that, the vibration of breakking away on the direction identical with liquid flow direction of the described stream wall that carries out active vibration.

6. fine-grain manufacturing apparatus as claimed in claim 3 is characterized in that, the described stream wall that carries out active vibration has piezoelectric element, described piezoelectric element in the surface-coated of that side that contacts with liquid insulating materials.

7. as each the described fine-grain manufacturing apparatus in the claim 3～6, it is characterized in that described fine-grain manufacturing apparatus is as emulsifier unit.

8. fine-grain manufacturing apparatus as claimed in claim 7 is characterized in that, described device a plurality of described fluid devices that have been connected in parallel.

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