WO1999015252A1 - Module de desaeration - Google Patents

Module de desaeration Download PDF

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Publication number
WO1999015252A1
WO1999015252A1 PCT/JP1997/003332 JP9703332W WO9915252A1 WO 1999015252 A1 WO1999015252 A1 WO 1999015252A1 JP 9703332 W JP9703332 W JP 9703332W WO 9915252 A1 WO9915252 A1 WO 9915252A1
Authority
WO
WIPO (PCT)
Prior art keywords
permeable membrane
gas permeable
degassing module
region
vacuum
Prior art date
Application number
PCT/JP1997/003332
Other languages
English (en)
Japanese (ja)
Inventor
Youichi Inoue
Yasuhiro Yoshimura
Yoshishige Endo
Yukiko Ikeda
Toshihiko Ariyoshi
Original Assignee
Hitachi, Ltd.
Nitto Denko Corp.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hitachi, Ltd., Nitto Denko Corp. filed Critical Hitachi, Ltd.
Priority to PCT/JP1997/003332 priority Critical patent/WO1999015252A1/fr
Priority to JP51878699A priority patent/JP3340444B2/ja
Publication of WO1999015252A1 publication Critical patent/WO1999015252A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0031—Degasification of liquids by filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • 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
    • 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
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties

Definitions

  • the present invention relates to a degassing module for removing gas dissolved in water using a gas permeable membrane.
  • water contains gases such as nitrogen and carbon dioxide in addition to oxygen, and water containing these dissolved gases often has an adverse effect.
  • gases such as nitrogen and carbon dioxide in addition to oxygen
  • water containing these dissolved gases often has an adverse effect.
  • water used in foods and pharmaceuticals has a high dissolved oxygen content, which promotes its decay and deterioration, pure water used in semiconductors produces oxide residues on the wafer, It also becomes a factor promoting corrosion of the weld.
  • a degassing method for removing dissolved gas in water using a hydrophobic membrane having a gas permeable function has been put to practical use.
  • water flows on one side of a membrane that has a gas transmission function but does not allow liquid to pass through, and only the dissolved gas in the liquid is reduced to the decompression side by depressurizing the opposite side of the membrane.
  • the gas is evacuated and degassed.
  • this gas permeable functional membrane is formed into a hollow tube, and a bundle is used in a decompression chamber and used as a degassing module.
  • a porous hollow membrane is used as a gas permeable functional membrane (hereinafter also referred to as a permeable membrane).
  • a permeable membrane gas permeable functional membrane
  • the larger the pore diameter formed in the permeable membrane the higher the deaeration efficiency, water leaks directly from the pores, and what permeates as water vapor condenses into water, resulting in leakage.
  • liquids such as chemicals or acids or alkaline liquids are used, there is a danger that the vacuum chamber or vacuum pump will corrode due to water leakage.
  • Reference 1 Japanese Patent Application Laid-Open No. 8-141372 (hereinafter referred to as Reference 1).
  • the inventor of the present application has conducted intensive studies to realize a deaeration module having high deaeration performance and no water leakage, and as a result, has reached the present invention.
  • the present inventor has conducted various experiments to improve the gas adhesion to the gas permeable membrane.
  • the reforming method for introducing appropriate roughness to a surface having a small surface energy for the following reasons. Is important.
  • Equation (1) holds in any case. By transforming this equation, equation (2) is obtained.
  • Fluorine resin has a relatively small surface energy
  • CF 2 which is the basic molecular structure of PTFE has a value of 18 dyne / cm, which is smaller than that of glass or metal.
  • FIG. 1 This effect can be basically explained by capillary action.
  • FIG. 1 we consider the case of a solid surface with a contact angle of 0 or more than 90 ° to water, and the case where there are three types of holes with different cylindrical hole diameters and a relationship of dl>d2> d3.
  • the pore size is sufficiently large, water can penetrate into the pores, and the dissolved gas can be converted to gas and adhere to the surface only at the corners of the pore grooves.
  • the hole diameter in the figure is close to the water droplet radius determined by the surface tension of water as shown by d2, water does not penetrate into the hole, and the dissolved gas changes to gas and many gases are removed. It can be attached to the surface.
  • the pore diameter is very fine as shown by d3
  • water does not enter the pore due to the effect of surface tension, but the volume of gas that can be adsorbed is small, and degassing efficiency cannot be improved.
  • the size of the pores is made appropriate and the adsorptivity to the permeable membrane surface and its By increasing the volume, high performance degassing efficiency can be realized as a result.
  • An appropriate value of the size of the hole is calculated by the following calculation. It is assumed that there is a cylindrical hole with a diameter d deep enough in the gas permeable membrane, and that water contacts the surface at a contact angle of zero. Considering the surface tension of water, the water pressure as P, and the balance of force at the water interface inside the hole,
  • the water inlet pipe is used at less than 6 atm, and the pressure difference is 1 to 7 atm because the outside of the permeable membrane tube is evacuated. If the pressure difference is 1 atm, the surface tension of water is 72 dyn / cm 2 , and the contact angle is 130 °,
  • a hole shape with a diameter of 0.3 to 11.3 zm is effective, and if possible, it is formed with fine projections such that the convex part becomes small, and parentheses are used. It is desirable that this is uniform over the entire surface. Although this figure focuses on the diameter of the hole, it is desirable that the surrounding edge be as small as possible. Therefore, the ideal shape is one having a pore diameter equivalent to d 2, and its edge is formed of a water-repellent substance that resembles water in the shape of a fine projection.
  • FIG. 3 schematically shows a cross section of this surface shape.
  • each triangle has one vertex. Therefore, the density of the vertices per unit area corresponds to 2.6 ⁇ 10 13 / m 2 to 1.8 ⁇ 10 10 / m 2 .
  • the surface treatment method for a gas-permeable membrane according to the present invention is a method for forming fine projections by physical collision when ions of high energy energy are injected into the surface of the gas-permeable membrane. Using a permeable membrane, a very high-performance degassing module can be realized.
  • FIG. 1 is a schematic diagram showing a relationship between a contact angle of a liquid in contact with a solid surface of a gas permeable membrane and a surface energy.
  • FIG. 2 is a schematic diagram showing a degassing rate when holes having different diameters are present on the gas permeable membrane surface.
  • FIG. 3 is a schematic cross-sectional view of a gas permeable membrane in which the degassing rate is maximized.
  • FIG. 4 is a scanning electron micrograph of the initial state of the fluororesin surface.
  • FIG. 5 is a scanning electron micrograph of a gas permeable membrane surface obtained by modifying the fluororesin surface by ion implantation according to Example 1 of the present invention.
  • Fig. 6 is a side photograph showing the water contact angle on the fluororesin surface in the initial state. is there.
  • FIG. 7 is a side view photograph showing the water contact angle of the surface of the fluororesin modified by ion implantation according to Example 1 of the present invention.
  • FIG. 8 is a cross-sectional view of a gas permeable membrane tube of the degassing module according to Embodiment 1 of the present invention.
  • FIG. 9 is a cross-sectional view of the gas permeable membrane tube of the degassing module according to Embodiment 1 of the present invention.
  • FIG. 10 shows the measurement results of the characteristics of the deoxidation efficiency of the degassing module according to the present invention.
  • FIG. 11 shows the results of measuring the water vapor leakage characteristics of the degassing module according to the present invention.
  • FIG. 12 is a scanning electron micrograph of a gas permeable membrane surface obtained by modifying the fluororesin surface by ion implantation according to Example 1 of the present invention.
  • FIG. 13 is a side view photograph showing the water contact angle of the surface of the fluororesin modified by ion implantation according to Example 2 of the present invention.
  • FIG. 14 is a cross-sectional view of a gas-permeable membrane tube of a degassing module according to Embodiment 3 of the present invention.
  • FIG. 15 is a sectional view of a degassing module according to Embodiment 3 of the present invention.
  • Figure 4 shows a scanning electron microscope surface photograph of the PTFE (polytetrafluoroethylene) used for the gas permeable membrane before reforming, and shows the PTFE gas permeable membrane after reforming by ion injection used in this example.
  • Fig. 5 shows a photograph
  • Table 1 shows the results of the measurement of surface roughness change
  • Figs. 6 and 7 show photographs showing their water contact angles.
  • FIG. 8 is a cross-sectional view
  • FIG. 9 is a cross-sectional structure of the deaerated module.
  • Fig. 10 shows the basic performance of the degassing module using this gas permeable membrane, as a result of examining the relationship between the degassing efficiency and the processing flow rate. Is shown in Fig. 11.
  • non-porous PTFE (having small pores through which gas molecules can pass) PTFE is used as the resin to be ion-implanted, and argon gas is ionized on this surface, and the acceleration voltage is 30 kV.
  • the implantation dose is about 10 14 ions / cm 2 .
  • the injection time is 60 seconds.
  • Figures 4 and 5 show scanning electron micrographs (SEM) before and after injection of Arion into PTFE. The initial state is a surface where the injection-molded product remains in the form of a film by mechanical grinding, so there are only a few flat and random holes.
  • Ra was roughened to the initial 0.09 sn force and 0.23 ⁇ m due to the modification of the ion injection, and the maximum surface roughness Rmax was also increased to 0.92 / m force and 2.02 m.
  • the variation of Ra ranged from 0.2 ⁇ m to 2 ⁇ m in the part with roughness such as scratches.
  • the shape at that time is a fine beard (needle) near the top as shown in the photograph shown in Fig. 5, and most of its length is more than 0.3 mm and locally long. It was 1.5 m, which was about 0.4 m on average.
  • the average distance between adjacent whiskers formed by ion implantation was 1.1 / m.
  • Fractal dimension is an expression method that quantifies the geometrical complexity of a surface. It takes 2.0 for a perfectly smooth surface, but this dimension increases as the three-dimensional complexity increases. For rough surfaces, the maximum is 3.G. The analysis result was 2.02 on average in the result before reforming. On the other hand, after the modification, there was slight variation depending on the measurement surface, and the average value increased significantly to 2.66, indicating that the surface shape was complicated.
  • this shape is not a hole but a protrusion on the surface, it changes to a hole shape as it goes inside, and is considered to be substantially equivalent to the hole shape described above. Also, the size of the projections was almost ideal as described above in terms of size.
  • a water drop of 0.005 ml was dropped on the surface, and the contact angle was measured.
  • Fig. 8 shows a photograph before reforming by ion implantation
  • Fig. 9 shows a photograph after reforming.
  • the water contact angle in the initial state of PTFE is 110 °, but the contact angle on the surface that has been modified by ion implantation to form fine protrusions reaches about 170 °. And had an extremely high water-repellent surface. In other words, it was confirmed that the surface had a shape to which gas could easily adhere.
  • FIG. 8 is a cross-sectional view showing a state in which the gas permeable membrane is formed in a tubular shape.
  • the influent 1 containing dissolved oxygen flows inside the gas permeable membrane tube 4 from left to right in the figure, but since the outside of the tube is almost vacuum, the dissolved oxygen in the liquid becomes gas bubbles 8 And a part thereof adheres to the inner wall of the gas permeable membrane tube 4.
  • the attached oxygen permeates through the permeable membrane, penetrates to the outside of the tube, and is released, so that the liquid is deoxygenated.
  • FIG. 9 is a cross-sectional view of a deoxygenating module configured so that a large number of liquids can be processed per unit time by bundling the gas permeable membrane tubes 4 into a module.
  • a pump for evacuating is installed outside the evacuation port 9 in the figure, and a vacuum of about 60 Torr to 260 Torr is maintained.
  • the performance of such equipment it is important to determine the amount of the processing liquid to achieve the predetermined degassing efficiency and at the same time how little water leakage occurs.
  • the characteristics at the beginning of the process are important. Specifically, the performance is determined by the film thickness, area, and content of the gas permeable membrane.
  • a degassing module with a gas permeable membrane thickness of 0.1 mm, a total tube area of 1.3 m 2 , and a total content of 260 cm 3 was prepared and its performance was compared.
  • the vacuum section is a single-unit vacuum pump.
  • the test was conducted in an environment with a temperature of about 20 ° C, pulled down to 60 (8. OkPa) Torr.
  • the degassing efficiency was calculated using the dissolved oxygen concentration C 0 of the completely treated liquid using a dissolved oxygen meter, and measuring the initial oxygen concentration C 1 at which the liquid started to flow.
  • the degassing module characteristics show that when the processing flow rate is 100 ml / min, the degassing efficiency is as high as 93%, Flow rate
  • the water vapor pressure indicating the amount of water leak was measured in one vacuum chamber.
  • the steam pressure was as high as 2.2 Torr when the processing flow rate was 100 ml / min, and as high as 3. OTorr when the processing liquid flow rate was 400 ml / min.
  • the characteristics of the degassing module when using the gas permeable membrane treated by ion injection shown in the examples are as follows: when the processing flow rate is 100 ml / min, the steam pressure is as low as 0.8 Torr and the processing liquid flow rate is 40 Even at Oml / min, it was not so high as 1.0 Torr, and it was found that the water leak could be maintained at a low level of about 1/3 while the degassing efficiency was high. On the other hand, the oxygen concentration was 2 to 4 Torr, which was higher than the partial pressure of water vapor.
  • the present embodiment when dissolved oxygen in the liquid becomes bubbles, it easily adheres to the surface of the permeable membrane, and the adhered gas is immediately sucked into the vacuum chamber through the permeable membrane, so that a very high deaeration efficiency is achieved. Since the water vapor component is obtained and is in contact with the liquid only at the tip of the protrusion on the surface of the permeable membrane, it is difficult for the water vapor component to be degassed to the outside. Further, according to the present embodiment, the surface of the inner peripheral surface of the pipe that comes into contact with the flowing liquid is a gas layer, so that the flow resistance of the degassing module can be extremely reduced. In this example, PTFE was used as the gas permeable membrane.
  • the element to be ion-implanted into the resin is a high-energy energy, which is a constraint, but the implanted ions remain in the resin without being exposed to the surface, so almost all elements are implanted.
  • the accelerating voltage is 5 kV or more, and if it is 40 kV, the melting of the resin starts, so this range is necessary.
  • the implantation dose is preferably 10 13 to 10 16 ions / cm 2 , and preferably 10 14 to 10 15 ions / cm 2 .
  • the injection time is within 1 to 100 seconds.
  • Example 2 will be described with reference to FIGS. 10 to 13 and Table 1.
  • FIG. As the gas permeable membrane, PFA with a thickness of 100 ⁇ m was used, and nitrogen gas was ionized into the membrane, and the acceleration voltage was injected at 8 kV.
  • the implantation dose is about 10 14 ions / cm 2 .
  • the injection time is 30 seconds.
  • the protrusion interval was about 0.8 ⁇ m, which was within the range deduced from the theoretical formula described above. The results are shown in Table 1 (above).
  • the center line average roughness Ra was increased from the initial 0.09 ⁇ m to 0.26 / m, and the maximum surface roughness Rmax was also changed from 0.92 ⁇ m to 1.78; .
  • the shape at that time was a fine beard near the top, as shown in the photograph shown in Fig. 5.
  • the fractal dimension analysis result increased from 2.02 before reforming to 2.40 due to reforming, and the water contact angle was measured to be about 156 °, confirming that the surface had high water repellency. It was done. That is, it was confirmed that the shape was such that gas easily adhered.
  • the basic performance of the degassing module of this example using this gas permeable membrane was measured under the same test conditions as in Example 1, and the results are also shown in FIGS. 10 and 11.
  • the degassing module characteristics when using an unprocessed PTFE gas permeable membrane were such that when the processing flow rate was 100 ml / min, the degassing efficiency was as low as 45%, and the processing liquid flow rate was limited.
  • the degassing module characteristics show that the degassing efficiency is as high as 93% when the processing flow rate is 100 ml / min, and the processing liquid flow rate is high. It was found that very high deaeration efficiency could be achieved without dropping even at 400 ml / min.
  • the degassing module characteristics using the gas permeable membrane treated by ion implantation shown in the present example are as follows. At n, the steam pressure is as low as 1.lTorr, and even when the processing solution flow rate reaches 400ml / min, it does not increase as much as 1.4Torr, and the degassing efficiency is high and the water leak is as low as about 1/2 It turned out that the state could be maintained.
  • the present embodiment when dissolved oxygen in the liquid becomes bubbles, it easily adheres to the surface of the permeable membrane, and the adhered gas is immediately sucked into the vacuum chamber through the permeable membrane, so that a very high deaeration efficiency is achieved.
  • the water vapor component is hardly degassed to the outside because it is in contact with the liquid only at the tip of the protrusion on the surface of the permeable membrane. This has the effect of providing a degassing module with very good characteristics. Further, in this embodiment, since low energy and short processing time are required, an effect that is excellent in mass production industrially can be expected.
  • Embodiment 3 will be described with reference to FIGS. 14 and 15.
  • the cross section is a concentric donut shape. Therefore, the outer surface of the inner tube 10-2 of the double gas permeable membrane tube is also subjected to the same surface treatment as in the first embodiment. Since this inner tube is connected to the vacuum chamber, the degassing efficiency can be further improved.
  • the length of the tube can be shortened, so that an extremely small module can be realized.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Physical Water Treatments (AREA)

Abstract

Selon l'invention, un film perméable aux gaz, dont la surface présente une faible énergie et une rugosité appropriée, est utilisé dans un module de désaération qui est exempt de fuite d'eau et présente un grand pouvoir de désaération. Ce film perméable aux gaz peut être produit par implantation d'ions dans la surface.
PCT/JP1997/003332 1997-09-19 1997-09-19 Module de desaeration WO1999015252A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP1997/003332 WO1999015252A1 (fr) 1997-09-19 1997-09-19 Module de desaeration
JP51878699A JP3340444B2 (ja) 1997-09-19 1997-09-19 脱気モジュールの製造方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP1997/003332 WO1999015252A1 (fr) 1997-09-19 1997-09-19 Module de desaeration

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003062422A (ja) * 2001-08-27 2003-03-04 Inst Of Physical & Chemical Res 気体分離膜及びその製造方法
JP2007144310A (ja) * 2005-11-28 2007-06-14 Shimadzu Corp 気液分離チップ、その製造方法及びそれを用いた全有機体炭素測定装置
WO2012023300A1 (fr) * 2010-08-18 2012-02-23 三菱重工業株式会社 Dispositif d'aération et système de désulfuration par eau de mer des gaz de combustion équipé de ce dispositif d'aération
US20150007721A1 (en) * 2011-12-13 2015-01-08 Sartorius Stedim Biotech Gmbh Hydrophobic or Oleophobic Microporous Polymer Membrane with Structurally Induced Beading Effect
JP2021015111A (ja) * 2019-07-11 2021-02-12 株式会社ニシヤマ 液中微粒子計測システムおよび脱気器
WO2023074670A1 (fr) * 2021-10-29 2023-05-04 株式会社クラレ Membrane poreuse et procédé de fabrication de membrane poreuse

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03169304A (ja) * 1989-11-28 1991-07-23 Nitto Denko Corp スパイラル型脱気膜モジュール
JPH07288710A (ja) * 1994-04-15 1995-10-31 Nec Corp ビデオ信号の水平方向拡大回路
JPH09155169A (ja) * 1995-12-07 1997-06-17 Junkosha Co Ltd 気体透過性膜

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03169304A (ja) * 1989-11-28 1991-07-23 Nitto Denko Corp スパイラル型脱気膜モジュール
JPH07288710A (ja) * 1994-04-15 1995-10-31 Nec Corp ビデオ信号の水平方向拡大回路
JPH09155169A (ja) * 1995-12-07 1997-06-17 Junkosha Co Ltd 気体透過性膜

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003062422A (ja) * 2001-08-27 2003-03-04 Inst Of Physical & Chemical Res 気体分離膜及びその製造方法
JP2007144310A (ja) * 2005-11-28 2007-06-14 Shimadzu Corp 気液分離チップ、その製造方法及びそれを用いた全有機体炭素測定装置
WO2012023300A1 (fr) * 2010-08-18 2012-02-23 三菱重工業株式会社 Dispositif d'aération et système de désulfuration par eau de mer des gaz de combustion équipé de ce dispositif d'aération
JP2012040494A (ja) * 2010-08-18 2012-03-01 Mitsubishi Heavy Ind Ltd エアレーション装置及びこれを備えた海水排煙脱硫装置
US20150007721A1 (en) * 2011-12-13 2015-01-08 Sartorius Stedim Biotech Gmbh Hydrophobic or Oleophobic Microporous Polymer Membrane with Structurally Induced Beading Effect
JP2015505725A (ja) * 2011-12-13 2015-02-26 ザルトリウス ステディム ビオテック ゲーエムベーハー 構造的に誘導されるビーディング効果を有する疎水性又は疎油性の微孔性高分子膜
US9364796B2 (en) 2011-12-13 2016-06-14 Sartorius Stedim Biotech Gmbh Hydrophobic or oleophobic microporous polymer membrane with structurally induced beading effect
JP2021015111A (ja) * 2019-07-11 2021-02-12 株式会社ニシヤマ 液中微粒子計測システムおよび脱気器
WO2023074670A1 (fr) * 2021-10-29 2023-05-04 株式会社クラレ Membrane poreuse et procédé de fabrication de membrane poreuse

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