JPS62140609A - Filtration separator - Google Patents

Abstract

PURPOSE:To easily and efficiently separate concrete components from a suspension contg. high-mol.wt. substances as solutes by filtering the suspension while forming a flow of the suspension parallel to the tubular filter surface. CONSTITUTION:A columnar body 2 is provided in a porous tubular body 1 while keeping a constant clearance with the main tube body, a part of the suspension 3 is filtered to the outside of the tubular body 1 as a filtrate 4 while the suspension flows through the clearance between the tubular body 3 and the columnar body 2, and the suspension flows out as a concentrate 5 from the opposite side. Meanwhile, the outside of the porous tubular body can be used as a filter surface. The thickness of the clearance used as the passage is preferably controlled to 0.1-10mm. Consequently, concrete components can be easily and efficiently separated from the suspension contg. high-mol.wt. substances as solutes. The separator is disassembled after use, various chemicals are added to the clogged tubular body which is then heated, hence the tubular body is regenerated, and then the separator is assembled and can be reutilized.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a filtration separation device. More specifically, it is used in various industrial fields including the food and pharmaceutical industries, which require the separation of suspended components from suspensions containing various high molecular weight substances as solutes, such as microorganisms, cells, and their constituents. The present invention relates to a filtration separation device used.

[Conventional technology] In the food and pharmaceutical industries, low molecular weight substances produced in fermenters, culture tanks, reactors, etc. are combined with tangible substances such as microorganisms, cultured cells, unreacted solids, and foreign substances. separation is taking place. Conversely, when obtaining microorganisms and cells as products, separation is performed for the purpose of separating them from the culture medium and removing waste products that inhibit their growth. A method for separating each particle component from such a suspension, that is, a suspension containing particles with a molecular weight of 1,000 to 20 (l) 0,000 as a solute, and further containing particles with a size of 1 to 1) μm. Mainly used methods include centrifugation, depth filtration, precision filtration, and ultrafiltration.

In the depth filtration method, a thick fibrous sheet or mat made of asbestos, filter paper, glass fiber, etc. is used as a filter medium, and the suspended components in the suspension are divided into 1. ! Separation is performed by trapping in Murayama.

The precision filtration method and the ultrafiltration method are surface filtration methods in which removal is mainly performed on the filter surface, and the former allows for more accurate separation than the depth filtration method.

Ultrafiltration uses semipermeable membranes made of various gel materials, etc.
A colloidal solution that is difficult to filter is filtered by applying pressure.

[Problems to be solved by the invention] Centrifugation is a method often used to clarify such suspensions, but it requires relatively large equipment for large-scale processing, and it is difficult to use a continuous processing system. The problem is that it is cumbersome to incorporate and is susceptible to contamination during separation.

The depth filtration method has drawbacks such as the carcinogenicity of asbeth l~, which is widely used as a filter medium, leakage of the filter medium, poor separation accuracy, and the need for filter aids.

Filtration separation methods such as precision filtration and ultrafiltration have been increasingly used in recent years, especially for internal diameters of 0.5 mm to l,
The use of a capillary-like filtration membrane of about 0 mm is considered advantageous because a large filtration area can be obtained with a small volume and the device can be made compact.

! -However, since the membranes used are limited to organic polymer materials, they have low heat resistance and durability, and
Since the iI structure cannot be decomposed, clogging on the surface of the filtration membrane cannot be sufficiently removed using various chemicals or heating, resulting in a short service life. Furthermore, machining of the end face for holding the capillary may be difficult depending on the material, and the materials that can be used are limited. Filters made of various inorganic materials such as ceramics and metals have extremely high heat resistance, and when treated at high temperatures, clogging organic matter can be completely removed by incineration, which has the advantage of a long lifespan. However, because it could not be processed into the thin hollow fiber shape shown above, only inefficient filtration devices could be obtained.

[Means for solving the problem] It has become clear that the problems seen in the suspension clarification method can be solved by using a porous tubular body as a filtering medium and setting it as follows. .

That is, a structure is installed inside or outside a porous tubular body to form a gap through which the suspension can move, and the suspension is used as a flow path to flow the suspension substantially parallel to the tubular body. A portion of the suspension is passed through a porous tubular body to perform filtration separation.

Although various types of structures can be considered, for example, columnar bodies or cylindrical bodies are installed in parallel at intervals on the inside or outside of the porous tubular body. The porous tubular bodies and their columnar or cylindrical structures have structures that can be easily disassembled and assembled, and the flow formed by combining porous tubular bodies of various shapes and columnar or cylindrical bodies. Provides the ability to change the thickness of the road. By using the filtration separation device configured in this way, the formed components can be easily and efficiently separated from a suspension containing a high molecular weight substance as a solute. Further, after use, the device can be disassembled, the clogged tubular body can be regenerated by applying various chemicals and heat treatment, and it can be reused by reassembling it.

[Function] In order to perform filtration separation of a suspension containing a high molecular weight substance as a solute, it is necessary to remove the filtration surface from the filtration surface, since in the total filtration method in which filtration is performed perpendicularly to the filtration surface, the filtration surface is rapidly clogged with suspended particles. The Talos flow filtration method, which performs filtration while forming parallel suspension flows, is effective.

This is because forming a flow along the filter surface has the effect of reducing the accumulation of suspended particles, and the faster the flow velocity with respect to the filter surface, that is, the higher the cross-sectional velocity, the higher this effect.

In order to increase this speed, it is effective to increase the flow rate per unit time or to decrease the channel thickness. However, until now, there has been no structure that takes this point into consideration using a porous tubular body as a filter medium.

FIG. 1a shows the basic concept of the present invention when the inside of a porous tubular body is used as a filtration surface. A columnar body 2 is installed in the porous tubular body 1 so as to maintain a constant gap from the tubular body, and while the suspension 3 flows through the gap between the tubular body 1 and the columnar body 2, a part of the suspension 3 becomes a filtrate 4. The suspension is filtered to the outside of the tubular body 1 and flows out as a concentrated liquid 5 from the opposite side. b
In this case, the outside is used as the filtering surface, and the suspension 3 is flowed into the gap between the outside of the tubular body 1 and the cylindrical body 6 installed on the outside, and the filtrate 4 flows into the inside of the tubular body 1. .

The thickness of the gap used as a flow path is 0.1 mm-1
0 mm, preferably 0.511111 to 5 nua.

As mentioned above, the thinner the channel thickness, the higher the effect of preventing clogging of the filter surface, but when it is less than 0.1111 m, there is a high possibility that suspended particles will clog the channel, and pretreatment is required. Moreover, since the flow path resistance becomes large, the liquid feeding pressure becomes high, which is not preferable. When the diameter is 10 mm or more, the amount of liquid required to feed to obtain a high flow rate increases, so the power cost required for liquid feeding increases, and the efficiency of filtration deteriorates.

Various types of suspensions to be filtered have various properties, and in order to achieve more effective filtration, it is desirable to appropriately set the rupture speed and the pressure involved in filtration, that is, the diaphragm pressure difference.

As for these setting ranges, the cutting speed is 100 to 1
0000 sec, diaphragm pressure difference, that is, suspension inflow pressure Pi of the filtration separation device, suspension outflow pressure Po, filtrate outflow pressure F
The relationship between o is (Pi + P o ) / 2- F o≦2
．． 0 Kg/cm" is preferable. If the shear velocity is less than 11]θ, the effect of preventing particles from sticking will not be obtained; if it is more than 000, if the suspension contains cellular components, This is undesirable as it may cause destruction.If the diaphragm pressure difference is 2°OK g/cm" or more,
The adhesion force of the suspended particles to the membrane surface becomes large, making clogging more likely to occur. The fact that the channel thickness is variable facilitates this setting and allows application to a wide range of suspensions. In order to make the above effect more effective, the average pore size should be 0,
It is preferable to use a porous tubular body having a diameter of 01 to 10 μm and a porosity of 15 to 80%. When the average pore diameter is 0.01 μm or less or the porosity is 15% or less, the filtration rate decreases and is not practical, and when it is 10 μm or more, particle removal accuracy deteriorates. Moreover, if the porosity is 80% or more, the strength of the porous body decreases, which is not preferable.

Note that the pore size here was determined from the trapping efficiency of polystyrene latex beads with uniform particle size (Uniform Latex Particles°' by Dow Chemical Company).

That is, a solution diluted to a solid content concentration of 0.1 wt'g is 10
01 to pass through and find the capture efficiency using the following formula.

Capture efficiency (%) = (Cf-Cp)/CfxlOOCf:
Latex concentration of stock solution Cp: Latex concentration of filtrate.

This trapping efficiency is determined starting from particles with a smaller particle size, and the particle size when this value reaches 100% is taken as the pore size. Moreover, the porosity was determined by the following formula.

Porosity (%) = pore volume f / porous body volume × I00 Materials for the porous tubular body include organic polymer materials such as fluorine-based and olefin-based materials, and ceramics such as aluminum oxide and silicon nitride. Any porous material may be used as long as it is made of an inorganic material such as a metal such as stainless steel, or a mixture of both materials, but in the filtration separation device of the present invention, an inorganic material such as a ceramic or a metal is particularly suitable. It is valid. This is because filters using these inorganic materials can only be formed into thin hollow fibers like those seen with organic polymer materials, resulting in poor filtration efficiency. The present invention has made it possible to obtain a filter that overcomes these drawbacks and is efficient, heat resistant, and durable.

Being able to easily disassemble each component makes it possible to sufficiently heat and chemically treat the filter medium, making it easy to remove clogging and regenerate the filter medium. Although fluorine-based organic polymer materials are superior in terms of durability against chemicals such as acids and alkalis, they cannot be used for long periods of time.
Deterioration is inevitable. Ceramic has excellent durability in this respect and can withstand high temperatures of 1000°C or higher, making it extremely useful for completely incinerating and removing organic substances that have caused clogging.

In order to further enhance the effect of preventing suspended particles from adhering to the filtration surface, it is also preferable to form irregularities on the surface of the porous tubular body, columnar body, or cylindrical body. This generates turbulence in the flow and utilizes the j11 separation effect of particles due to this.
1. It is also effective to form uniform convex portions of 0 mm or to form spiral concave portions of similar height.

The porous tubular body of the filter medium can be installed in multiple tubes,
It is also preferable to fill the inside and outside of the porous tubular body with granular structures in order to increase the filtration efficiency.

Furthermore, by bundling a plurality of these tubular bodies described above in parallel, it is also possible to set up an apparatus capable of processing a larger amount.

The present invention will be explained in more detail by examples below.
The examples are not intended to limit the invention.

[Example] Figure 2 shows an example of a filtration separation device that uses a circular tubular porous body and flows a suspension inside the porous body.
A fixing gasket 12 is fitted on both ends of the tube 1, and an inner tube 13 with threads cut at both ends is fixed from the outside of the fixing gasket 12 with a set screw 14 to hold it inside the porous tube 11, and the tube with a flow path 15 formed therein is removed. It is set in the tube 16. The suspension '<'& 17, which is the filtration stock solution, is introduced from the input port 1.18, enters the inside of the porous tube 11 through the slit 19 provided in the set screw 14, and flows in parallel through the channel 15. It flows out from the opposite side. Filtration is performed while flowing through the channel 15,
The filtrate generated outside the porous tube 11 flows out from the filtrate outlet 20. The thickness of the flow path 15 can be easily changed by changing the outer diameter of the inner tube 13.

FIG. 3 similarly shows an embodiment of an apparatus that uses a circular tubular porous body and allows a suspension to flow outside.

Fixing gaskets 22 are attached to both ends of the porous tube 21,
It is set in the outer cylindrical tube 25 with a set screw 24 via a spacer 23. The gap between the outer cylindrical tube 25 and the circular tube 21 becomes a flow path. The robot 2 enters the outer tube 25 in the tangential direction of this tube.
6 and 27 are installed in the outlet port 1, and the suspension is introduced into the circular tube 21 from 26 in the tangential direction, moves through the flow path 28 while flowing spirally along the surface of the circular tube, and then passes through the outlet port 27. More leakage. During this time, a portion of the suspension is filtered through the circular tube, and a clarified filtrate is obtained from the filtrate boat 29.

Next, an example of an experiment conducted to confirm the effects of the present invention will be shown.

Experimental example 1 Average pore diameter 0.5μm, inner diameter 15m+n, outer diameter 19mm
Inside a ceramic porous pipe with a length of 250 mm,
A filtration and separation device having the structure shown in FIG. 1 was prepared by installing a cylinder with an outer diameter of 13 mm. Using this filtration device, an experimental circuit as shown in FIG. 4 was constructed and a circulation experiment was conducted. The test suspension is introduced from the suspension storage tank 31) by a circulation pump 32 into a dess 1-filtration device 33, through which it is returned to 31 again. Pressure gauges 35 are installed at the inlet, outlet, and filtrate sides of the filtration device, and filtration conditions are set by controlling the regulating valve 36 and filtrate pump 34. The suspension in the suspension storage tank 31 was stirred by a magnetic stirrer 37. The obtained filtrate is again 31
However, by switching the switching valve 38, the filtrate is collected from the three filtrate collection ports into the measuring device 40,
The amount of filtration is measured each time. As a suspension, glucose 20g, peptone 20g, yeast extract 10g
Alcohol yeast was cultured in a medium prepared by dissolving the following in 1 liter of water. The filtration conditions are a circulation flow rate of 300 m1. The diaphragm indenter was set at 0 and 3 K g/cm2. In addition, the bacterial weight was adjusted to 5% (wet weight). Similarly, a comparative example was assembled in which no cylinder was placed inside the porous circular tube.

Experimental example 2 Average pore diameter 0.1 μm, inner diameter 20 mm, outer diameter 23 mm,
A filtration device was prepared using a ceramic porous circular tube with a length of 150 mm as a filter medium and installed in an outer cylinder with an inner diameter of 24 mm as shown in FIG. 2. Using the same circuit and suspension as in Experimental Example 1, circulation flow rate 80 m1/min, diaphragm indenter
The experiment was carried out at 0.04 g/cm".

As a comparative example, a similar tube with one end sealed and a filtrate outlet formed at the other end was prepared, and was directly placed in a suspension storage tank to perform filtration. In this comparative example, two methods were used: one in which filtration was carried out continuously at a constant pressure, and the other in which backwashing was repeated by applying pressure in the opposite direction for 1 minute every 10 minutes.

Experimental Results Figure 5 shows the results of Experimental Example 1. In the example, there was no change in the filtration flow rate even 20 hours after the start of the filtration experiment, and filtration was performed stably, but in the comparative example, the filtration rate gradually decreased and the filtration surface became clogged. It is expected that

This difference was particularly remarkable in Experimental Example 2, and as shown in Figure 6, in the example, 75% of the initial flow rate, or approximately 3 ml/min, was maintained even 5 days after the start of filtration, but continuous In the comparative example in which filtration was performed, clogging occurred rapidly and almost no filtrate could be obtained. Even when backwashing was performed, the flow rate was less than half of the initial flow rate on the second day.

Also, although not shown in the figure, in Experimental Example 1, after the experiment, the filtration device was disassembled, the porous tube was treated and regenerated in an electric furnace at 1200°C, and the same experiment was repeated 10 times, or the initial filtration rate was No strange [Hi] was seen.

[Effects of the Invention] As described above, the filtration separation device according to the present invention has the following advantages.

(D) Since the thickness of the flow path from the filtration surface of the porous tubular body is regulated, the efficiency of filtration is improved, clogging is less likely to occur, and precision filtration of suspensions can be performed for a long time.

(■ The components of the filtration device are easy to disassemble and assemble, and the flow path can be appropriately set according to the properties of the suspension.

(2) Since the components of the filtration device are easy to disassemble and assemble, clogged or clogged filter media can be regenerated by performing various treatments such as chemicals and heat.

(2) Porous tubular bodies made of various materials can be used depending on the conditions of the stock solution to be filtered.

[Brief explanation of drawings]

FIGS. 1a and 1b show the basic concept of the present invention, and FIGS. 2 and 3 are partial sectional views of the embodiment. FIG. 4 shows an experimental circuit, and FIGS. 5 and 6 show the results. I...Porous tubular body 2...Columnar body 3...Suspension liquid 4...Filtrate 5...Concentrate liquid
6... Cylindrical body 11... Porous tube 12
... Fixed gasket 13 ... Inner pipe 14
... Set screw 15 ... Channel 16 ...
・Outer cylinder 17...Suspension liquid 18...Lobo l to 19...Sleeve I section 20...Filtrate outlet 21...Porous tube 22...Fixed gasket 23...・Spacer 24... Set screw 25... Outer tube 26... Inlet boat 27... Outlet boat 28... Channel 29.
・・Filtrate port

Claims (8)

[Claims] (1) Consisting of a porous tubular body and a structure that forms a gap inside or outside of the tubular body through which fluid can move, and uses the gap as a flow path to direct fluid to the tubular body. A filtration separation device characterized in that the flow is substantially parallel to a porous tubular body, and at least a portion of the flow is passed through a porous tubular body to perform filtration separation. (2) The filtration separation device according to claim 1, wherein the gap has a thickness of 0.1 mm to 10 mm. (3) The filtration separation device according to claims 1 and 2, wherein the structure is a columnar body or a cylindrical body installed in parallel with a gap inside or outside the porous tubular body. (4) A porous tubular body and a columnar body or a cylindrical body installed in parallel with a gap inside or outside the porous tubular body can be easily replaced or assembled, and the thickness of the gap is variable. A filtration separation device according to any one of claims 1 to 3, characterized in that: (5) Claims 1 to 4 characterized in that the columnar body or the cylindrical body has irregularities formed on its surface.
The filtration separation device described in Section 1. (6) The filtration and separation device according to any one of claims 1 to 5, wherein the porous tubular body has irregularities formed on its surface. (7) The filtration separation device according to any one of claims 1 to 6, wherein the porous tubular body has an average pore diameter of 0.01 to 10 μm. (8) The filtration separation device according to any one of claims 1 to 7, wherein the porous tubular body is made of an inorganic material.