WO2013031968A1 - 中空糸膜モジュールの検査方法 - Google Patents
中空糸膜モジュールの検査方法 Download PDFInfo
- Publication number
- WO2013031968A1 WO2013031968A1 PCT/JP2012/072213 JP2012072213W WO2013031968A1 WO 2013031968 A1 WO2013031968 A1 WO 2013031968A1 JP 2012072213 W JP2012072213 W JP 2012072213W WO 2013031968 A1 WO2013031968 A1 WO 2013031968A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- hollow fiber
- fiber membrane
- membrane module
- potting end
- damaged
- Prior art date
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- 238000004382 potting Methods 0.000 claims abstract description 86
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
- B01D65/102—Detection of leaks in membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
- B01D65/106—Repairing membrane apparatus or modules
- B01D65/108—Repairing membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/21—Specific headers, end caps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/90—Additional auxiliary systems integrated with the module or apparatus
- B01D2313/903—Integrated control or detection device
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2315/00—Details relating to the membrane module operation
- B01D2315/06—Submerged-type; Immersion type
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules
Definitions
- the present invention generally relates to a method for inspecting a hollow fiber membrane module, and in particular, specifies a position of a damaged hollow fiber membrane (damaged membrane) in a bundle of hollow fiber membranes constituting the hollow fiber membrane module. It relates to the inspection method.
- Membrane separation that separates a substance from a liquid by a separation membrane (filtration membrane) has features such as energy saving, space saving, labor saving, and product quality improvement, and is therefore used in various fields. Specifically, membrane separation using a microfiltration membrane or an ultrafiltration membrane is used in a water purification process for producing industrial water or tap water from river water, groundwater or sewage treated water.
- a separation means used for performing membrane separation there is a hollow fiber membrane module provided with a hollow fiber membrane bundle obtained by bundling hollow fiber membranes in which a large number of pores are formed on a side wall.
- the hollow fiber membrane module can take a large membrane area per unit volume, it can be used in many fluid processing fields, for example, concentration and desalting of enzymes by ultrafiltration membranes, production of water for injection, and recovery of electrodeposition paints. It is used for final filtration of ultrapure water, treatment of sewage wastewater, turbidity of river water, lake water, and underground water, chemical purification by microfiltration membrane, sterilization, turbidity, etc.
- the hollow fiber membrane module is roughly classified into a pressure type hollow fiber membrane module and an immersion type hollow fiber membrane module.
- the pressurized hollow fiber membrane module filters raw water by introducing pressurized raw water into the inside of each hollow fiber membrane constituting the hollow fiber membrane bundle, and flowing the raw water from the inside to the outside through the side wall of the hollow fiber membrane.
- the submerged hollow fiber membrane module sucks the open end of the hollow fiber membrane in a state where the hollow fiber membrane bundle is immersed in the tank containing the raw water, and flows the raw water from the outside to the inside through the side wall of the hollow fiber membrane.
- This is a type of hollow fiber membrane module that filters raw water and obtains permeated water (filtered water) inside the hollow fiber membrane.
- the pressure type hollow fiber membrane module can set the filtration pressure higher than the immersion type hollow fiber membrane module, so the processing amount per membrane area is large, so the number of membranes required for the treatment can be reduced and the installation area It has the advantage that it can be made smaller.
- the submerged hollow fiber membrane module performs filtration by immersing the hollow fiber membrane bundle in raw water, so it is excellent in discharging turbidity clogged between the membranes, and membrane filtration can be performed even in high turbid raw water. Since the filtration method is simple and there are few incidental pipes, there are advantages such as reduction in equipment costs.
- the hollow fiber membrane bundle of the hollow fiber membrane module is usually configured by bundling thousands to tens of thousands of elongated hollow fiber membranes, and each hollow fiber membrane in the hollow fiber membrane bundle functions as a filtration membrane. .
- each hollow fiber membrane in the hollow fiber membrane bundle functions as a filtration membrane.
- a damaged hollow fiber membrane (damaged membrane) in the hollow fiber membrane bundle unfiltered raw water or insufficiently filtered water is mixed in the filtered water, and filtration with a desired quality is performed. Water will not be obtained. Therefore, it is necessary to detect the presence and position of a damaged membrane, which is a damaged hollow fiber membrane, in order to obtain filtered water (permeated water) having a desired quality.
- Patent Document 1 For example, by detecting the bubbles released from the open end of the damaged membrane by imaging the end face of the hollow fiber membrane bundle while pressurizing the gas in contact with the outside of the hollow fiber membrane bundle and processing the obtained image
- Patent Document 1 There is a method (Patent Document 1) for specifying a hollow fiber membrane from which bubbles are released as a damaged membrane. Further, the hollow fiber membrane at the position where the end of the hollow fiber membrane module is scanned with the laser beam while the gas containing the fine particles flows inside the hollow fiber membrane module outside the hollow fiber membrane, and the laser beam collides with the fine particles and is scattered.
- Patent Document 2 for determining a film as a damaged film
- Patent Document 3 an inspection method for identifying a damaged membrane that is damaged and causes a leak by changing the range in which the pressurized gas is fed from the end face of the hollow fiber membrane module or repeating the detection operation while narrowing down
- JP 2007-17171 A Japanese Patent No. 3319825 JP 2009-78243 A
- Patent Document 1 requires a sophisticated pressurized container for installing the hollow fiber membrane module therein, and has a problem of an apparatus.
- the method of patent document 2 is a structure which specifies the position of the damaged hollow fiber membrane based on the supplemented scattered light in addition to the need for a pressurized container, the accuracy of position specification is not high. There was a problem.
- the method of Patent Document 3 is complicated in that it is necessary to narrow down the inspection area, and further, it takes time until detection as it becomes the center of the end face. Even if the area is narrowed down, the range is detected. There was a problem that the position of the damaged hollow fiber membrane could not be narrowed down sufficiently due to the tool.
- the present invention has been made to solve the above-described problems, and is a hollow fiber membrane module capable of quickly specifying the position of a damaged membrane in the hollow fiber membrane module with a simple configuration.
- the purpose is to provide an inspection method.
- a method for inspecting a hollow fiber membrane module Forming a sealed space on the potting end surface by covering the potting end surface with a translucent cap on the potting end surface where the open end of the hollow fiber membrane of the hollow fiber membrane bundle constituting the hollow fiber membrane module is open; Filling the liquid inside the hollow fiber membrane and depressurizing the sealed space in a state where the outside of the hollow fiber membrane is in contact with air; and Detecting bubbles released from the potting end face; Irradiating the potting end surface with two line-shaped light rays longer than the diameter of the potting end surface through the translucent cap so that the bubbles on the potting end surface intersect with each other; Identifying the position on the potting end face of the hollow fiber membrane that is damaged using the intersection of the two line-shaped rays; Providing leakage prevention to the damaged hollow fiber membrane, An inspection method for a hollow fiber membrane module is provided.
- the position of the damaged hollow fiber membrane can be specified by a simple operation of irradiating two line-shaped light beams on the potting end surface.
- Locating the damaged hollow fiber membrane comprises: A step of attaching a pair of marks on each of the line-shaped light beams while irradiating the line-shaped light beams on the line-shaped light beams that are opposed to each other across the potting end surface in the radial direction of the potting end surface. When, Removing the cap from the potting end face; A step of connecting a pair of marks for each line-shaped light beam with a line and reproducing an intersection of the lines as a position of the damaged hollow fiber membrane.
- the specifying step is a step of irradiating two line rays again so as to match the respective pairs of marks, and specifying the intersection as the position of the damaged hollow fiber membrane.
- the two line-shaped light beams are applied to the potting end face in a state of being orthogonal to each other.
- Scales are arranged at regular intervals on the transparent cap transparent side.
- the step of preventing leakage includes the step of applying a repair agent to the hollow fiber membrane specified as the damaged hollow fiber membrane.
- the step of preventing leakage is performed while performing the step of irradiating the two line-shaped light beams and specifying the intersection point as the position of the damaged hollow fiber membrane.
- the linear light beam is constituted by a laser beam having a wavelength of 500 nm or more and 690 nm or less.
- the repair agent comprises an adhesive having a combined curing function of moisture curing and UV curing.
- the hollow fiber membrane module is an immersion type hollow fiber membrane module.
- An inspection device for a hollow fiber membrane module A decompression means for decompressing the potting end face where the open end of the hollow fiber membrane of the hollow fiber membrane bundle constituting the hollow fiber membrane module is open; Irradiating means for irradiating two linear rays that are longer than the diameter of the potting end surface intersecting the potting end surface; The irradiation means can independently change the irradiation position on the potting end face of the two line-shaped light beams, A hollow fiber membrane inspection device is provided.
- An object of the present invention is to provide a hollow fiber membrane module inspection method and repair method that can quickly identify the position of a damaged membrane in the hollow fiber membrane module with a simple configuration.
- the hollow fiber membrane module in which the damaged membrane is specified and repaired by the inspection method of the hollow fiber membrane module 1 of the present embodiment, sucks the open end of the hollow fiber membrane while being immersed in a tank containing raw water.
- This is a so-called submerged hollow fiber membrane module that obtains permeated water (filtered water) inside the hollow fiber membrane.
- the inspection object of the inspection method and apparatus of the present invention is not limited to the above-described immersion type hollow fiber membrane module, and other types of hollow fiber membrane modules are also objects of the present invention.
- FIG. 1 is a drawing schematically showing the main part of the hollow fiber membrane module 1.
- the hollow fiber membrane module 1 is composed of a thin cylindrical hollow fiber membrane 2 in which a large number of pores are formed on the side wall, and adhesives are attached to both ends of a bundle of cylindrical hollow fiber membrane bundles 4 bundled in hundreds to tens of thousands.
- 6 is a module having a fixed structure.
- the hollow fiber membranes 2 are bonded and fixed to each other by an adhesive 6 with one end of the potting end face 8 being open and the other potting end face 9 being closed. Yes.
- the present invention can also be applied to a hollow fiber membrane module having a structure in which the hollow fiber membrane 2 is bonded and fixed with both ends opened.
- the membrane filtration operation of the hollow fiber membrane module 1 is performed in a vertical arrangement, that is, an arrangement in which each hollow fiber membrane 2 extends in the vertical direction.
- the present invention is also applicable to a submerged hollow fiber membrane module in which a membrane filtration operation is performed in a horizontal arrangement, that is, an arrangement in which each hollow fiber membrane extends in the horizontal direction.
- the hollow fiber membrane 2 is the same as a known hollow fiber membrane, and the material thereof is not particularly limited as long as it is a porous hollow fiber membrane.
- a thread membrane is preferred. From the viewpoint of membrane strength, a polyvinylidene fluoride hollow fiber membrane is more preferable.
- the diameter of the pores provided on the side wall of the hollow fiber membrane 2 is, for example, in the range of 0.001 ⁇ m to 1 ⁇ m.
- the outer diameter of the hollow fiber membrane 2 is not particularly limited, but is preferably in the range of 250 ⁇ m to 3000 ⁇ m because the hollow fiber membrane 2 has high oscillating properties and excellent detergency.
- the material of the adhesive 6 that bonds and fixes the hollow fiber membranes 2 at both ends of the hollow fiber membrane bundle 4 is not limited, but is preferably a thermosetting resin such as an epoxy resin or a urethane resin.
- a hollow space is formed on one end side of the hollow fiber membrane bundle so as to form a sealed space with the potting end surface 8 on one end side that is bonded and fixed with the end of the hollow fiber membrane 2 open.
- a removable bottomed cylindrical transparent cap 10 is fitted (FIG. 2).
- the transparent cap 10 is a bottomed cylindrical member, and the internal space communicates with an external suction means via the suction port 12 so that the suction can be performed under reduced pressure.
- an access port for injecting a repair agent may be provided on the side surface of the transparent cap 10.
- the transparent cap 10 is made of a transparent or translucent material as a whole so that bubbles discharged from the opening end of the damaged film can be visually recognized from the outside during the specific operation of the damaged film.
- Transparent or translucent glass or a synthetic resin material is used, but it is preferable to use a thermoplastic resin material to which bubbles do not easily adhere.
- the transparent cap 10 is made of polyvinyl chloride, methyl methacrylate resin, polystyrene resin, fluorine resin, polycarbonate, polysulfone, polyethersulfone, acrylonitrile-styrene copolymer, acrylonitrile-butadiene copolymer, It is preferably made of polychlorofluoroethylene or the like.
- inspection may be sufficient.
- the position of the damaged film is determined by using two orthogonal line-shaped laser beams (cross lines) 14 and 16 longer than the diameter of the potting end face 8. Mark.
- a laser projector 18 that irradiates two orthogonal line-shaped laser beams (cross lines) 14 and 16 onto the potting end surface 8 (end surface on the filtration side) of the hollow fiber membrane bundle 4 has a potting end surface 8. Is disposed above. The irradiation positions of the line laser beams 14 and 16 are movable on the potting end surface 8.
- the laser projector 18 used as the light source one that can generate the line-shaped laser beams 14 and 16 with high visibility is preferable, and one that generates a laser beam having a wavelength in the visible light region is selected.
- the laser light generated from the laser projector 18 has a wavelength in a region exceeding 450 nm, which is a cured region of the ultraviolet curable resin. In the infrared region exceeding 700 nm, laser light cannot be visually observed, which is not preferable. Therefore, the laser projector 18 that generates a line laser beam having a wavelength of 500 nm or more and less than 690 nm is preferable. Specifically, a laser projector 18 that generates red laser light having a wavelength of 635 nm or green light having a wavelength of 532 nm is used.
- the hollow fiber membrane module 1 is fixed to a vertical arrangement in which the potting end surface 8 where the end of the hollow fiber membrane 2 is open is upward using a fixture or the like.
- This fixing method is not particularly limited.
- a transparent cap 10 is put on the potting end face 8 of the hollow fiber membrane bundle 4.
- the transparent cap 10 has a bottom surface separated from the potting end surface 8 of the hollow fiber membrane bundle 4 so that a sealed space is formed between the transparent cap 10 and the potting end surface 8 of the hollow fiber membrane bundle 4. It is fitted to the tip of the.
- the inner peripheral surface of the open end of the transparent cap 10 and the outer peripheral surface of the distal end portion of the hollow fiber membrane bundle 4 are connected in an airtight state, and the inside of the transparent cap 10 is a sealed space.
- Each hollow fiber membrane 2 of the hollow fiber membrane module 1 is filled with a liquid such as water in the internal space, and the outer periphery is surrounded by air, that is, the outside is in contact with air.
- a hydrophilic treatment is performed by wetting the inside of the hollow fiber membrane with ethanol or the like so that the water content of the hollow fiber membrane is reduced. The state that has entered inside. Furthermore, in order to facilitate the visual recognition of bubbles for inspection, it is preferable to supply a small amount of water into the transparent cap 10 to form a water layer having a thickness of about several millimeters on the potting end face 8.
- the transparent cap 10 is put on one potting end surface. Then, the other potting end surface is covered with a member such as rubber or a film in order to maintain airtightness, and the opening is temporarily sealed, so that the gas that has entered the inner space of the hollow fiber membrane is allowed to enter from the other potting end surface. Avoid leakage.
- the space in the transparent cap 10 is decompressed by decompression means (not shown).
- decompression means not shown.
- the hollow fiber membrane 2 is filled with a liquid such as water, the surrounding air enters the internal space from the pores of the peripheral wall due to the surface tension of the liquid if there is no breakage.
- the damaged (defect) portion communicates with the outside air, so that air enters the internal space of the hollow fiber membrane 2 from the damaged portion by decompression.
- the breakage refers to a state in which the membrane is cut off, a state in which a pinhole that cannot maintain the filtration capability is caused by a flaw or the like.
- the air that has entered the internal space of the hollow fiber membrane 2 becomes bubbles and rises in the liquid in the hollow fiber membrane 2, and from the opening end of the hollow fiber membrane 2 that opens at the potting end surface 8, the transparent cap 10 Released into a covered space. Therefore, by visually recognizing this bubble from the outside of the transparent cap 10, the position of the damaged hollow fiber membrane, that is, the damaged membrane can be detected.
- the intersection 19 of the two line-shaped laser beams 14 and 16 is arranged at the place where the bubble is generated on the potting end face 8, and the line laser beams 14 and 16 extending outside the potting end face 8.
- Marks 20, 22, 24, and 26 are attached on the extended portion (protruding portion). That is, a total of four places and two pairs of marks 20, 22, 24, and 26 are attached to each of the line-shaped laser beams 14 and 16, one on each side of the potting end face 8 (FIG. 4).
- a pair of marks 20, 22 are positioned on the line-shaped light beam opposed to the line-shaped laser beam 16 on the line-shaped light beam facing the potting end surface 8 on the radially outer side of the potting end surface 8.
- a pair of marks 24 and 26 are attached to the positions on the line-shaped light beams that are opposed to each other across the potting end surface 8 on the radially outer side of the potting end surface 8.
- the marking locations are two points facing each other in the radial direction across the potting end face 8 with respect to one line-shaped laser, and two line-shaped lasers are irradiated per damaged site.
- paper or the like is placed at a position near the outer side of the outer edge of the potting end surface 8 or an outer position of the potting end surface, and marking is performed on the paper.
- a ruler such as a scale may be provided at regular intervals on the inner or outer circumference of the transparent cap, and may be used to assist marking.
- FIG. 5 is an example of the transparent cap 10 having a scale S on the outer periphery.
- the ruler As a ruler (ruler) provided inside the transparent cap, protrusions at regular intervals or a transparent ruler are provided on the inner wall of the position where the laser beam is transmitted and serve as a guideline for the extension line of the laser beam. Is mentioned.
- the ruler provided on the outside of the transparent cap includes paper that is printed on the outside of the transparent cap with grid-like lines printed, and markings are made at the intersections of the lattice printed on this paper and the laser. Is given.
- each pair (20, 22) (24, 26) of the mark located across the potting end face 8 is connected by a line, and the intersection point is reproduced on the potting end face 8, and the position is specified as the position of the damaged film. To do.
- a repair agent is attached to the end of the damaged hollow fiber membrane so as to block the opening of the hollow fiber membrane so that raw water does not flow into the hollow fiber membrane.
- a repair agent having a moisture curing function is preferable. This is because the hollow fiber membrane module 1 in a wet state can be repaired without drying, and since it reacts with the moisture contained in the hollow fiber membrane and cures, it exhibits an anchor effect and adheres well to the hollow fiber membrane. It is.
- a conventional repairing agent made of an ultraviolet curable resin or a hot melt resin that can be cured only by ultraviolet rays can also be used.
- the repair agent at the repaired portion has a high degree of crosslinking, and does not swell or deteriorate even when immersed in water after curing, and is excellent in strength and durability.
- a repair agent having a photo-curing function refers to a repair agent capable of maintaining a practical strength even after the ultraviolet ray irradiation is stopped after the curing starts by UV irradiation and curing progresses to a practical strength. Those having characteristics such as curing in seconds after irradiation with ultraviolet rays are preferred.
- a repair agent having a photocuring function a repair agent containing a photopolymerization initiator having a reaction wavelength between 100 and 400 nm and capable of avoiding the influence of visible light (indoor scattered light) is preferable.
- LED ultraviolet light which is commonly used as an ultraviolet irradiation device, has the largest amount of light in the vicinity of 350 nm, and such a repair agent including a photopolymerization initiator having a maximum absorption in the vicinity of 350 nm is efficient, cost and resource-saving. From the viewpoint of, it can be preferably used.
- a one-pack type repairing agent excellent in pot life is preferable from the viewpoint of workability, for example, an acrylic adhesive, an epoxy adhesive, an oxetane adhesive, a cyanoacrylate adhesive, etc.
- the repair agent which is the object of the present invention can be obtained by adding a composite curing function to them.
- the leak is detected while the periphery of the leaked part is at least wet without drying the hollow fiber membrane module after the leak test.
- a repair agent is attached so as to block the part.
- the adhesion method include a method of dripping a repair agent and a method of applying it.
- the repairing agent adheres well to the periphery of the leaked part due to the anchor effect caused by the reaction with the moisture in the hollow fiber membrane, and the internal region is sufficiently cured by irradiation with ultraviolet rays. Therefore, the repair agent at the repaired portion has strength and durability due to the anchor effect and a high degree of crosslinking, and does not swell or deteriorate even if it is immersed in the water tank to be treated again.
- the “periphery of the leak portion” means a portion where the repair agent adheres for the purpose of closing the leak portion.
- the ultraviolet irradiation device in addition to the LED ultraviolet lamp (UV-LED) described above, for example, a metal halide lamp, a high-pressure mercury lamp, an ultra-high pressure mercury lamp, a deep ultraviolet lamp, a lamp that excites a mercury lamp from the outside without electrodes using a microwave, Examples include ultraviolet lasers and xenon lamps.
- UV-LED LED ultraviolet lamp
- a metal halide lamp for example, a high-pressure mercury lamp, an ultra-high pressure mercury lamp, a deep ultraviolet lamp, a lamp that excites a mercury lamp from the outside without electrodes using a microwave
- Examples include ultraviolet lasers and xenon lamps.
- an LED ultraviolet lamp using a UV-LED as a light source is easier to switch between lighting (irradiation) and extinguishing than, for example, other ultraviolet lamps. Therefore, in the repair work in which turning on (irradiating) and turning off is repeated, it is preferable to easily control the timing of ultraviolet irradiation.
- the viscosity of the repair agent before curing affects the workability of the repair.
- the preferred viscosity of the repairing agent varies depending on the size of the leaking part and can be used from 1 mPa ⁇ s to a paste at room temperature (23 ° C.), preferably 10 to 3000 mPa ⁇ s, more preferably 100 ⁇ 1000 mPa ⁇ s. If the upper limit of this range is exceeded, even if a repair agent is attached to the periphery of the leaked portion 30 in a wet state, it will not easily penetrate in the film thickness direction, and therefore it will be difficult to react with moisture in the film, resulting in poor anchoring effect. It tends to be sufficient.
- the repair agent penetrates too much around the leaked part, resulting in a part where the light (ultraviolet rays) irradiated at the time of curing is difficult to reach, and unreacted components remain. There is a possibility that the hole of the part which does not need repairing is blocked with a repairing agent and the membrane area is reduced.
- an ethyl cyanoacrylate photocurable instant adhesive containing a photoinitiator having an absorption maximum at 365 nm is preferred.
- the repair may be completed by removing the transparent cap and applying and curing a repair agent in a state where the laser beam is irradiated.
- the curing wavelength is different from the laser beam for specifying the location, so that the work can be performed without being cured even during the coating operation.
- the repair agent is cured by performing UV irradiation again.
- the line-shaped laser beams are preferably arranged so as to be orthogonal to each other, but it is possible to identify a leak location by marking at least four locations even if they are not orthogonal.
- two laser beams such as a cross-line laser are orthogonal to each other.
- at least two line laser beams intersect each other, for example, even if they intersect at an acute angle of 60 ° C.
- two straight lines can be defined, and since there is only one intersection of the two straight lines, it is possible to identify the damaged portion. .
- the line-shaped laser beam is preferably irradiated perpendicularly to the potting end face 14, but may be irradiated from an oblique direction.
- Example 1 As a hollow fiber membrane module, an immersion type hollow fiber type microfiltration membrane module manufactured by Mitsubishi Rayon Co., Ltd. (Sterapore LFB3423, membrane area 50 m2, MF module using a hydrophilic PE hollow fiber membrane, nominal pore size 0.1 micron) was prepared. One hollow fiber membrane in the hollow fiber membrane bundle of this hollow fiber membrane module was damaged (damaged), and this hollow fiber membrane module was used as a hollow fiber membrane module to be inspected.
- each hollow fiber membrane is filled with water
- a transparent cap is fitted to the end portion of the hollow fiber membrane bundle that is a water collecting portion of the hollow fiber membrane module.
- a small amount of water is supplied into the cap so that the potting end surface of the hollow fiber membrane bundle is covered with water.
- This hollow fiber membrane module was oriented in the vertical direction in the air, and the inside of the transparent cap was decompressed to about ⁇ 20 kPa by a vacuum pump. As a result, bubbles were generated from the open end of the damaged hollow fiber membrane.
- Red crossline laser projector placed 1m above the potting end face of the hollow fiber membrane module Model: Z5RX-635 (Tsuruga Denki Co., Ltd., wavelength 635nm, laser output 5mW x 2), two orthogonal crossline lasers was irradiated to the end face of the potting through the transparent cap. At this time, the two cross-line lasers are arranged so that the intersection thereof overlaps the bubble generation position on the potting end surface. And the cross-line laser marked two places, a total of four places which cross
- the decompression is stopped, the transparent cap is removed, the potting end of the hollow fiber membrane bundle of the hollow fiber membrane module is exposed, and the intersection of the crossline laser is reproduced from the four marking positions on the outer periphery of the potting end surface. The position of the open end of the damaged membrane was identified.
- UV curable instant adhesive (Loctite # 4305, manufactured by Henkel) was dropped as a repair agent at the position of the identified damaged film, and then UV light was irradiated and cured by LED type UV light (wavelength 375 nm). . Thereafter, a transparent cap was fitted to the end portion of the hollow fiber membrane module, and the internal space was decompressed to perform a leak test again.
- Example 2 The same process as in Example 1 was performed until the stage of specifying the position of the damaged film by irradiating the cross-line laser.
- Example 2 while continuously irradiating the damaged part with the loss line laser, the transparent cap was removed, and several ml of an ultraviolet curable instant adhesive (Loctite # 4305 manufactured by henkel) was dropped into the center of the irradiated cross line light. And cured with UV light. Thereafter, a transparent cap was fitted to the end of the hollow fiber membrane module again, and re-inspection was performed. As a result, generation of bubbles was not confirmed, and it was confirmed that the damaged hollow fiber membrane was sealed with the UV curable resin.
- an ultraviolet curable instant adhesive Lictite # 4305 manufactured by henkel
- Example 1 Comparative Example 1
- the leak location was detected under reduced pressure.
- the damaged part was marked on the transparent cap with oily magic by visual observation from above the transparent cap having an access port for repair on the side of the transparent cap.
- the repair agent was injected from the access port to the position corresponding to the marking position without removing the cap, and the repair was performed.
- the marking position and the repair agent injection position are liable to shift, and three injection operations are required to repair the damaged portion.
- Example 2 In the same manner as in Example 1, the leak location was detected under reduced pressure. A photo was taken from the top of the transparent cap to identify the location, and the leak location was repaired based on the photo, but it was difficult to identify and repair was done in 1.5 cm x 1.5 cm area units. I had to make it.
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Abstract
Description
中空糸膜モジュールは、単位体積あたりの膜面積を大きく採ることができることから、多くの流体処理分野、例えば、限外濾過膜による酵素の濃縮・脱塩、注射用水の製造、電着塗料の回収、超純水のファイナルフィルトレーション、下廃水処理、河川水・湖沼水・伏流水の除濁、精密濾過膜による薬品精製、除菌、除濁等に利用されている。
除去方法としては、中空糸膜モジュールの下部に空気を吹き込んで膜を水中で振動させることにより、中空糸膜の外表面に付着した不純物を除去する空気洗浄(空洗)、中空糸膜モジュールの濾過方向とは逆方向に、つまり中空糸膜の内側から外側に向けて高圧の水(逆洗水)を流し中空糸膜の外表面に付着した不純物を中空糸膜の内側から排除する逆圧水洗浄(逆洗)などが挙げられる。
したがって、損傷した中空糸膜である損傷膜の有無およびその位置を検出することが、所望の品質の濾過水(透過水)を得るために必要である。
さらに、微粒子を含む気体を中空糸膜のモジュール内で中空糸膜の外側に流しながら中空糸膜モジュールの端をレーザー光で走査し、レーザー光が微粒子と衝突して散乱した位置の中空糸膜を損傷膜と判定する方法(特許文献2)、
さらにまた、中空糸膜モジュールの端面から加圧気体を送り込む範囲を変更、又は絞り込みながら検出動作を繰り返すことにより、損傷してリークを発生させている損傷膜を特定する検査方法(特許文献3)が挙げられる。
また、特許文献2の方法は、加圧容器が必要であることに加え、補足した散乱光に基づいて損傷した中空糸膜の位置を特定する構成であるため、位置特定の精度が高くないという問題があった。
さらに、特許文献3の方法では、検査エリアを絞っていかなければならない点が煩雑であり、さらに、端面の中心部になるほど検出までの時間を要する、エリアを絞り込めてもその範囲は検出治具に制約され、損傷している中空糸膜の位置を十分に絞り込めないなどの問題があった。
中空糸膜モジュールの検査方法であって、
中空糸膜モジュールを構成する中空糸膜束の中空糸膜の開口端が開口しているポッティング端面に透光性のキャップを被せて前記ポッティング端面上に密閉空間を形成するステップと、
前記中空糸膜の内部に液体を充填し前記中空糸膜の外部が空気に接触した状態で、前記密閉空間を減圧するステップと、
前記ポッティング端面から放出された気泡を検出するステップと、
前記ポッティング端面の前記気泡が検出された位置で交差するように、前記透光性キャップ越しに前記ポッティング端面の直径より長い2本のライン状光線を前記ポッティング端面に照射するステップと、
前記2本のライン状光線の交点を利用して損傷している中空糸膜の前記ポッティング端面上での位置を特定するステップと、
前記損傷している中空糸膜にリーク防止を施すステップと、を備えている、
ことを特徴とする中空糸膜モジュールの検査方法が提供される。
前記損傷している中空糸膜の位置を特定するステップが、
前記ライン状光線を照射しながら、前記各ライン状光線に対し、前記ポッティング端面の径方向外方で前記ポッティング端面を挟んで対向する前記ライン状光線上に位置に対となったマークを付すステップと、
前記ポッティング端面から前記キャップを取り外すステップと、
前記ライン状光線毎に対となったマーク同士を線で結び、前記線の交点を前記損傷している中空糸膜の位置として再現するステップと、を備えている。
前記特定ステップが、前記各対のマークに合わせるように再度、2本のライン状光線を照射し、その交点を前記損傷した中空糸膜の位置として特定するステップである。
前記2本のライン状光線は、互いに直交した状態で前記ポッティング端面に照射される。
前記透明キャップ透明の側部に定間隔で目盛りが配置されている。
前記リーク防止を施すステップが、前記損傷している中空糸膜として特定された中空糸膜に補修剤を塗布するステップ、を備えている。
前記2本のライン状光線を照射し、その交点を前記損傷した中空糸膜の位置として特定するステップを行いながら、前記リーク防止を施すステップが行われる。
ライン状光線が、波長500nm以上690nm以下を有するレーザー光線によって構成されている。
前記補修剤が、湿気硬化及びUV硬化の複合硬化機能を有する接着剤からなる。
前記中空糸膜モジュールが浸漬型中空糸膜モジュールである。
中空糸膜モジュールの検査装置であって、
中空糸膜モジュールを構成する中空糸膜束の中空糸膜の開口端が開口しているポッティング端面を減圧する減圧手段と、
前記ポッティング端面に互いに交差する前記ポッティング端面の直径より長い2本のライン状光線を照射する照射手段と、を備え、
前記照射手段は、前記2本のライン状光線の前記ポッティング端面上での照射位置を、独立して変更可能である、
ことを特徴とする中空糸膜の検査装置が提供される。
先ず、本発明の好ましい実施形態の中空糸膜モジュールの検査方法によって損傷膜が特定され補修される中空糸膜モジュールについて説明する。
本実施形態の中空糸膜モジュール1の検査方法によって損傷膜の特定・補修が行われる中空糸膜モジュールは、原水を収容した槽内に浸漬した状態で、中空糸膜の開口端を吸引して中空糸膜の内側で透過水(濾過水)を得るタイプのいわゆる浸漬型中空糸膜モジュールである。
なお、本願発明の検査方法および装置の検査対象は、上記の浸漬型中空糸膜モジュールに限定されるものではなく、他のタイプの中空糸膜モジュールも本願発明の対象となる。
なお、本願発明は、両端が開口した状態で中空糸膜2が接着固定されている構造の中空糸膜モジュールにも適用可能である。
しかしながら、本願発明は、横置き配置すなわち各中空糸膜が水平方向に延びる配置で膜濾過運転が行われる浸漬型中空糸膜モジュールにも適用可能である。
例えば、ポリアクリロニトリル、ポリフェニレンスルフォン、ポリフェニレンスルフィドスルフォン、ポリフッ化ビニリデン、ポリプロピレン、ポリエチレン、ポリスルホン、ポリビニルアルコール、酢酸セルロースやセラミック等の無機素材からなる群から選ばれる少なくとも1種を含む材料から形成される中空糸膜であることが好ましい。膜強度の点から、ポリフッ化ビニリデン系中空糸膜であることがより好ましい。
また、中空糸膜2の外径も特に限定されないが、中空糸膜2の揺動性が高く、洗浄性に優れるため、250μm~3000μmの範囲内であることが好ましい。
本実施形態の検査方法では、中空糸膜2の端が開口した状態で接着固定されている一端側のポッティング端面8との間に密閉空間を形成するように、中空糸膜束の一端側に取外し可能な有底円筒状の透明キャップ10が嵌合させられる(図2)。透明キャップ10は、有底円筒状の部材であり、内部空間が吸引口12を介して外部の吸引手段に連通され、減圧吸引可能な構成とされている。さらに、透明キャップ10の側面には、補修剤注入のアクセスポートなどを設けても良い。
中空糸膜2の端が開口しているポッティング端面8に透明キャップ10を被せ、この透明キャップ内を、吸引口12等を介して減圧し、ポッティング端面から発生する気泡を検出することによって中空糸膜モジュール1の損傷膜を検出する中空糸膜モジュールの検査方法では、検出時にポッティング端面8が透明キャップ10内に配置されているため、ピンを打つ等して、気泡が発生している即ち損傷膜が存在している位置をマーキングすることができない。
本実施態様では、直交する2本のライン状レーザービーム(クロスライン)14、16を、中空糸膜束4のポッティング端面8(濾過側の端面)上に照射するレーザープロジェクタ18が、ポッティング端面8の上方に配置される。各ライン状レーザービーム14、16の照射位置は、ポッティング端面8上で移動可能とされている。
700nmを超える赤外線領域ではレーザー光を目視できないため好ましくない。したがって、500nm以上690nm未満の波長を有するライン状レーザービームを生成するレーザープロジェクタ18が好ましい。具体的には波長635nmの赤色、または波長532nmの緑色のレーザー光を発生させるレーザープロジェクタ18が使用される。
次に、本発明の好ましい実施態様の中空糸膜モジュールの検査方法である損傷膜特定方法について説明する。
まず、中空糸膜モジュール1を、固定具などを用いて、中空糸膜2の端が開口しているポッティング端面8が上方になる縦置き配置に固定する。なお、この固定方法は、特に限定されない。
さらに、検査に気泡の視認を容易にするために、少量の水を、透明キャップ10内に供給し、ポッティング端面8上に厚さ数mm程度の水の層を作ることが好ましい。
しかしながら、中空糸膜2に破断箇所があると、損傷(欠陥)箇所が外気と連通するので、減圧によって損傷箇所から空気が中空糸膜2の内部空間に侵入する。
このとき、2本のライン状レーザービーム14、16の交点19が、ポッティング端面8上の気泡が発生している部位(リーク箇所)に位置するように、各ライン状レーザービーム14、16の照射位置は調整される(図3)。
具体的にはポッティング端面8の外縁の外方側近傍位置あるいは、ポッティング端面の外方位置に紙などを配置しておき、この紙にマーキングを行う。
また、透明キャップの外側に設けられるルーラー(定規)としては、格子状の線が印刷され透明キャップの外側に配置された紙が挙げられ、この紙に印刷された格子とレーザーとの交点にマーキングが施される。
さらに、必要に応じて、損傷膜に補充剤を塗布して硬化させて損傷膜のリークを防止して、検査を完了させる。
本実施形態における中空糸膜モジュールの補修では、損傷している中空糸膜の端部に補修剤を付着させて中空糸膜の開口を塞ぎ、原水がその中空糸膜に流れ込まないにようしている。
(実施例1)
中空糸膜モジュールとして、三菱レイヨン社製の浸漬型の中空糸型精密濾過膜モジュール(ステラポアーLFB3423、膜面積50m2、親水性PE製中空糸膜使用MFモジュール、公称孔径0.1ミクロン)を準備した。この中空糸膜モジュールの中空糸膜束中の1本の中空糸膜を傷つけ(損傷させ)、この中空糸膜モジュールを検査対象の中空糸膜モジュールとした。
この中空糸膜モジュールを、空気中で上下方向に配向し、真空ポンプによって透明キャップの内部を-20kPa程度に減圧した。この結果、損傷させられた中空糸膜の開口端から気泡を生じた。
その後、中空糸膜モジュールの端部に透明キャップを嵌合させ、内部空間を減圧することにより、再度、リーク検査を行った。
(実施例2)
実施例2では、損傷部位にロスラインレーザーを引き続き照射しながら、透明キャップを外し、照射されているクロスライン光の中心に紫外線硬化型瞬間接着剤(henkel社製 Loctite #4305)数mlを滴下し、UVライトで硬化させた。
その後、再度、中空糸膜モジュールの端部に透明キャップを嵌合させ、再検査を行った。その結果、気泡の発生は確認されず、損傷した中空糸膜がUV硬化樹脂により封止されたことが確認された。
実施例1と同様に、減圧下でリーク箇所の検出を行った。
透明キャップ側面に補修のためのアクセスポートを有する透明キャップの上から目視によって、損傷箇所を透明キャップ上に油性マジックでマーキングした。さらに、キャップを外さずに、アクセスポートからマーキング位置に対応する位置に補修剤を注入して補修を行った。
しかしながら、マーキング位置と補修剤注入位置とがずれ易く、損傷箇所を補修するために、3回の注入作業が必要であった。
実施例1と同様に、減圧下でリーク箇所の検出を行った。その場所の特定のために透明キャップの上部から写真を撮影し、その写真を元にリーク箇所の補修を行ったが、特定することは難しく、1.5cm×1.5cmのエリア単位での補修にせざるを得なかった。
Claims (11)
- 中空糸膜モジュールの検査方法であって、
中空糸膜モジュールを構成する中空糸膜束の中空糸膜の開口端が開口しているポッティング端面に透光性のキャップを被せて前記ポッティング端面上に密閉空間を形成するステップと、
前記中空糸膜の内部に液体を充填し前記中空糸膜の外部が空気に接触した状態で、前記密閉空間を減圧するステップと、
前記ポッティング端面から放出された気泡を検出するステップと、
前記ポッティング端面の前記気泡が検出された位置で交差するように、前記透光性キャップ越しに前記ポッティング端面の直径より長い2本のライン状光線を前記ポッティング端面に照射するステップと、
前記2本のライン状光線の交点を利用して損傷している中空糸膜の前記ポッティング端面上での位置を特定するステップと、
前記損傷している中空糸膜にリーク防止を施すステップと、を備えている、
ことを特徴とする中空糸膜モジュールの検査方法。 - 前記損傷している中空糸膜の位置を特定するステップが、
前記ライン状光線を照射しながら、前記各ライン状光線に対し、前記ポッティング端面の径方向外方で前記ポッティング端面を挟んで対向する前記ライン状光線上に位置に対となったマークを付すステップと、
前記ポッティング端面から前記キャップを取り外すステップと、
前記ライン状光線毎に対となったマーク同士を線で結び、前記線の交点を前記損傷している中空糸膜の位置として再現するステップと、を備えている、
請求項1に記載の中空糸膜モジュールの検査方法。 - 前記特定ステップが、前記各対のマークに合わせるように再度、2本のライン状光線を照射し、その交点を前記損傷した中空糸膜の位置として特定するステップである、
請求項1に記載の中空糸膜モジュールの検査方法。 - 前記2本のライン状光線は、互いに直交した状態で前記ポッティング端面に照射される、
請求項1乃至3のいずれか1項に記載の中空糸膜モジュールの検査方法。 - 前記透明キャップ透明の側部に定間隔で目盛りが配置されている、
請求項1乃至4のいずれか1項に記載の中空糸膜モジュールの検査方法。 - 前記リーク防止を施すステップが、前記損傷している中空糸膜として特定された中空糸膜に補修剤を塗布するステップ、を備えている、
請求項1ないし5のいずれか1項に記載の中空糸膜モジュールの検査方法。 - 前記2本のライン状光線を照射し、その交点を前記損傷した中空糸膜の位置として特定するステップを行いながら、前記リーク防止を施すステップが行われる、
請求項3ないし6のいずれか1項に記載の中空糸膜モジュールの検査方法。 - ライン状光線が、波長500nm以上690nm以下を有するレーザー光線によって構成されている、
請求項1ないし7のいずれか1項に記載の中空糸膜モジュールの検査方法。 - 前記補修剤が、湿気硬化及びUV硬化の複合硬化機能を有する接着剤からなる、
請求項6ないし8のいずれか1項に記載の中空糸膜モジュールの検査方法。 - 前記中空糸膜モジュールが浸漬型中空糸膜モジュールである、
請求項1ないし9のいずれか1項に記載の中空糸膜モジュールの検査方法。 - 中空糸膜モジュールの検査装置であって、
中空糸膜モジュールを構成する中空糸膜束の中空糸膜の開口端が開口しているポッティング端面を減圧する減圧手段と、
前記ポッティング端面に互いに交差する前記ポッティング端面の直径より長い2本のライン状光線を照射する照射手段と、を備え、
前記照射手段は、前記2本のライン状光線の前記ポッティング端面上での照射位置を、独立して変更可能である、
ことを特徴とする中空糸膜の検査装置。
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EP12827748.0A EP2752234A4 (en) | 2011-08-31 | 2012-08-31 | METHOD FOR INSPECTING A HOLLOW FIBER MEMBRANE MODULE |
JP2012542055A JP5399568B2 (ja) | 2011-08-31 | 2012-08-31 | 中空糸膜モジュールの検査方法 |
US14/342,277 US20140216138A1 (en) | 2011-08-31 | 2012-08-31 | Inspection method of hollow fiber membrane module |
KR1020147003156A KR101431431B1 (ko) | 2011-08-31 | 2012-08-31 | 중공사막 모듈의 검사 방법 및 중공사막 모듈의 검사 장치 |
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JP7244310B2 (ja) * | 2018-03-14 | 2023-03-22 | 旭化成株式会社 | 中空糸膜モジュールのリーク試験方法、純水の製造方法及び純水の製造装置 |
JP2020131093A (ja) * | 2019-02-15 | 2020-08-31 | 野村マイクロ・サイエンス株式会社 | 注射用水の製造装置及び製造方法 |
CN110441217B (zh) * | 2019-08-30 | 2023-06-06 | 舟山市博远科技开发有限公司 | 一种砼试块的渗透单元及具有该渗透单元的测定仪 |
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US20140216138A1 (en) | 2014-08-07 |
JP5399568B2 (ja) | 2014-01-29 |
KR20140024967A (ko) | 2014-03-03 |
JPWO2013031968A1 (ja) | 2015-03-23 |
KR101431431B1 (ko) | 2014-08-18 |
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