WO2004086008A1 - Procede de mesure de la taille des pores d'un materiau filtrant poreux - Google Patents

Procede de mesure de la taille des pores d'un materiau filtrant poreux Download PDF

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Publication number
WO2004086008A1
WO2004086008A1 PCT/JP2004/003102 JP2004003102W WO2004086008A1 WO 2004086008 A1 WO2004086008 A1 WO 2004086008A1 JP 2004003102 W JP2004003102 W JP 2004003102W WO 2004086008 A1 WO2004086008 A1 WO 2004086008A1
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WO
WIPO (PCT)
Prior art keywords
filter
gas
pressure
gas flow
pore size
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PCT/JP2004/003102
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English (en)
Japanese (ja)
Inventor
Tomonori Takahashi
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Ngk Insulators Ltd.
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Publication date
Application filed by Ngk Insulators Ltd. filed Critical Ngk Insulators Ltd.
Publication of WO2004086008A1 publication Critical patent/WO2004086008A1/fr

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    • 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
    • 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
    • G01N2015/084—Testing filters

Definitions

  • the present invention provides a method for evaluating a filter related to the average pore diameter by applying a so-called bubble point method. More specifically, the present invention provides a pore size measurement method capable of evaluating a filter body related to an average pore size that is useful for practical use in a filter body in which pores of a ceramic body or the like are three-dimensionally complicated. . Background art
  • Evaluation of the average pore diameter of various filtration media is essential as evaluation of the basic performance, and various evaluation methods such as a bubble point method, a mercury method, and a bacterial filtration method have been conventionally performed. Above all, the bubble point method is widely used for quality control of various types of filtration media because of relatively simple measurement.
  • the measurement of the average pore diameter in this method is performed by: Using the assumption that the ratio of the amount of gas permeated through the body equals the ratio of the amount of permeated gas permeating through pores larger than the pore diameter corresponding to the gas pressure at each stage, with respect to the permeated gas permeating through all pores. (“ANUAL BOOK ⁇ F AMER I CAN STANDARDS” vo l. 1 1.01, AMER I CAN SOC I ETY FOR TEST I NG AND MATER I AL
  • a filter body not filled with the test liquid hereinafter referred to as “dry filter body” and a filter body filled with the test liquid (hereinafter referred to as “wet filter body”) are included.
  • dry filter body a filter body not filled with the test liquid
  • wet filter body a filter body filled with the test liquid
  • Each filter is placed on a holder with each end sealed, and a pressurized gas is supplied to one surface of each filter, and the pressure of the pressurized gas is increased step by step.
  • the amount of gas passing through each filter is detected, and the ratio of the gas flow rate passing through the wet filter to the gas flow rate passing through the dry filter (wet filter Z dry filter) corresponds to the gas pressure corresponding to 1Z2.
  • the pore diameter is regarded as the average pore diameter (MFPD), and is determined from the following equation (1).
  • MFPD is the average pore diameter ( ⁇ m)
  • 0 is the contact angle (°) of the test liquid filled in the pores of the filter with the material constituting the filter
  • ⁇ is the filtration Surface tension (NZm) of the test liquid filled in the pores of the body
  • B is a constant number of cavities (0.715) or 1
  • P is the gas passing through the wet filter relative to the gas flow through the dry filter
  • MPa gas pressure
  • 0 may usually approximate 0 degree.
  • the gas-liquid interface waits until the gas-liquid interface has sufficiently developed to the pore openings of the filter.
  • the gas flow path of the wet filter through which the gas passes is part of the gas through the dry filter. It is based on the assumption that it is the same as the transmission path.
  • the present invention has been made in view of the above-described problems, and can accurately and highly accurately measure an average pore diameter of a filter having three-dimensionally intricate pores. It is an object of the present invention to provide a method for measuring the pore size of a filter, which enables quality evaluation reflecting the performance of the filter. As a result of earnest studies to solve the above-mentioned problems, the present inventor has obtained the following knowledge regarding the point that an appropriate evaluation result could not be obtained by the conventional method.
  • the fluid to be filtered in the ordinary filtration flows in a distribution determined by the connection of the pores.
  • Fig. 6 (b) when the gas is passed through the wet filter sequentially from low pressure, the gas starts to permeate preferentially to large pores, which is different from normal filtration.
  • the fluid flow path of the filter is formed by the combination of a plurality of pores and is three-dimensionally complicated and intricate. However, it is easy to follow the path of gas permeation of the dry filter and a path that is significantly different from ordinary filtration.
  • gas permeation depends on one path determined by the gas flow rate.
  • the portion of the gas that enters through a certain pore always permeates through a particular path.
  • the gas pressure is maintained until the so-called saturation
  • the gas circulates largely, and the path through which the gas passes through the reference dry filter is different from the path through which the gas permeates through the wet filter. For this reason, in the conventional method, there is a difference in the actual evaluation target from the reference dry filter, which is a factor that further reduces the accuracy of the evaluation result.
  • the present invention provides a dry filter in a dry state, and a wet filter in which pores of the dry filter are filled with a test liquid, supplying a pressurized gas to each filter, The pressure is increased stepwise, the gas flow permeating through each filter is detected at each gas pressure step, and then the average pore diameter is calculated based on the following equation (1). If the fluid passage time (S) determined by the following formula (2) is less than 3 seconds, then (S) seconds to 30 seconds.
  • the fluid passage time (S) is 3 seconds or more
  • the present invention provides a method for measuring the pore diameter of a body.
  • MFPD is the average pore diameter ( ⁇ m)
  • 0 is the contact angle (°) of the test liquid filled in the pores of the filter with the material constituting the filter
  • a is the contact angle of the filter.
  • B is the capillary constant (0 ⁇ 15) or 1
  • P is the permeability of the wet filter to the gas flow through the dry filter.
  • the gas pressure (MPa) at which the gas flow ratio (wet filter / dry filter) becomes 12 is shown.
  • X is the thickness (m) of the filter in the filtration direction
  • J is the linear velocity (mZs) of the fluid to be filtered in practical use
  • Vs is the viscosity of the test liquid ( P a ⁇ s)
  • Vr is the viscosity (P a ⁇ s) of the fluid to be filtered.
  • the ratio of the gas flow rate passing through the wet filter to the gas flow rate passing through the dry filter is 15 to 1/2. It is preferably carried out in the range, more preferably in all gas pressure stages in this range.
  • the holding time of each gas pressure step in the range where the gas flow rate ratio is 15 to 1/2 is the average of the gas pressure steps in the range where the gas flow rate ratio is 1/5 to 12.
  • the holding time is preferably within 10% of the soil, and more preferably the holding time in the range where the gas flow rate ratio is 1Z5 to 1Z2 is 1 second to 1 minute.
  • the pressure value for increasing the pressure from one gas pressure step to the next gas pressure step is determined by a membrane when the fluid to be filtered is permeated at the linear velocity (J) of the fluid to be filtered in practical use. It is preferable that the pressure increase value is larger than the differential pressure, and each pressure increase value from one gas pressure step to the next gas pressure step in a range where the gas flow rate ratio is 1 to 5 to 1 Z 2 is It is further preferable that the average flow rate is within 20% of the soil in the range where the gas flow rate ratio is 1Z5 to 1/2. Further, it is preferable that each boosted value in the range where the ratio of the gas flow rates is 1Z5 to 12 is 0.01 to 0.04 MPa.
  • FIG. 1 is an explanatory diagram schematically showing the configuration of an apparatus for implementing the evaluation method of the present invention.
  • FIG. 2 is a cross-sectional view schematically showing a state in which a filter is installed on a holder in one example of the evaluation method of the present invention.
  • FIG. 3 is a graph showing the relationship between the gas flow rate and the gas pressure detected in each filter (dry filter, wet filter).
  • FIG. 4 is a graph showing the relationship between the average pore diameter and the gas pressure retention time obtained in each of the examples and comparative examples.
  • FIG. 5 is a graph showing the distribution of the average pore diameter when 22 samples were measured by the methods of Example 1 and Comparative Example 8.
  • Figs. 6 (a) and 6 (b) are explanatory diagrams schematically showing the presence of pores in a ceramic filter
  • Fig. 6 (a) is a schematic diagram of the flow of the fluid to be filtered in practical use
  • Fig. 6 (b) schematically shows the gas flow in the conventional measurement method.
  • FIG. 1 shows the flow of a measuring device that is usually used in the evaluation method of the present invention, and includes a pressurized gas supply source 11 and a pressure of a gas introduced from the pressurized gas supply source 11. Control, a pressure sensor 16 for measuring the pressure set by the relevant regulator 12, a holder 10 for installing the filter 2, and a gas flow supplied to the filter. And a flow meter 14 for measurement.
  • FIG. 2 is a cross-sectional view showing a state where the filter body 2 is installed in the holder 10.
  • Fig. 3 is a graph showing the relationship between the permeated gas flow rate and the gas pressure detected in each filter (dry filter and wet filter).
  • H in the graph indicates the permeate gas of the wet filter. It indicates the gas pressure at which the flow rate is 1 Z 2 with respect to the permeate gas flow rate of the dry filter.
  • the seal member 3 is a combination of a polymer such as epoxy or a glaze and a packing, a ring or the like. After measuring the gas permeation amount, install the wet filter 2 in which the pores of the same dry filter 2 are filled with the test liquid with the ends thereof similarly sealed in the holder 10 and measure the gas permeation amount. I do.
  • the filter 2 to be evaluated in the present invention is not particularly limited except that it is a porous body.
  • the filter 2 can be applied to various filter such as filter paper, an organic resin filter, and a ceramic filter.
  • the evaluation method of the present invention It can be particularly preferably applied to a filter body in which pores are complicated and complicated, and in this regard, application to a ceramics filter is preferable.
  • the present invention can also be applied to a ceramics filter in which one or more filtration membranes having different pore diameters are laminated on a porous base material.
  • a plate-shaped filter is shown in FIG. 2, a filter, such as a tube or a monolith, can be measured by preparing a holder.
  • test liquid 4 to be filled in the pores of the dry filter 2 examples include high-purity water, denatured alcohol, and mineral oil as described in D1129 and D1193 of ASTM F316-86. , 1,1,2-trichloro-1,2,2-toluolate, or a fluorine-based inert liquid (trade name: Florinato FC-140, a fluorine-based inert liquid manufactured by SLEM) is preferred.
  • examples of the fluid to be filtered that is to be filtered in actual use include water and petroleum.
  • a stepwise pressurized gas is supplied to one surface of the dry filter and the wet filter, and at this time, in the measurement of the permeated gas of the wet filter, each gas pressure step is measured. If the passage time (S) of the fluid to be filtered determined by the equation (2) is less than 3 seconds, (S) seconds to 30 seconds, and if the passage time (S) of the fluid to be filtered is 3 seconds or more, (S) After holding the wet filter at a constant pressure for a holding time of S) seconds to (SX 10) seconds, the pressure is increased to the next gas pressure stage.
  • the pore diameter can be measured accurately by setting the retention time to 10 times or less the passage time (S) of the fluid to be filtered. However, when (S) is shorter than 3 seconds, (S) Even if the retention time is 30 seconds or less even if the retention time exceeds 10 times, the pore size can be measured with good delicateness.
  • (S) obtained from Expression (2) depends on the linear velocity (J) of the fluid to be filtered in practical use, but (J) is usually used when designing a filtering device using the filtering body. It is set to a known value when the filter is manufactured considering its design. In addition, (J) may be set to have a predetermined width. In that case, (S) also has a predetermined width. In such a case, the above (S) is not more than 3 seconds. ) Max A value of 3 seconds or more and (S) less than 3 seconds means that the maximum value of (S) is less than 3 seconds. Then, the upper limit of the retention time is more likely to be higher when the maximum value is closer to the maximum value of (S), and is preferably 10 times or less, and more preferably 2 times or less, the maximum value of (S). '
  • the holding time is too short, the gas flow rate that should be detected in the pressurization stage is not detected, such as when the gas-liquid interface is moving in a long flow path. Will be smaller than the evaluation result. Therefore, the holding time must be longer than the value of (S). If (S) has a predetermined width, (S) here also means the maximum value. Further, if the holding time is too short, operability and responsiveness of the device will become problematic.
  • the retention time is longer than (S) and as short as possible therein, so that the filtration target fluid to be actually filtered is a filter.
  • the gas pressure is maintained for a time close to the time when the gas passes through. For this reason, the path of the gas in the wet filter is similar to the path through which the fluid to be filtered respectively passes, and the evaluation can sufficiently reflect the performance of the filter in actual use. Since the fluid to be filtered and the test liquid have different viscosities due to differences in viscosity, the time required to pass through the membrane and the time required for gas pressure discharge are different. Is corrected.
  • the gas pressure holding time in each gas pressure stage may be set to a range outside the above setting up to the gas pressure stage where the ratio of the gas flow rates is 1 to 5.
  • the gas pressure holding time in each gas pressure stage should be as small as possible in order to perform accurate and precise evaluation. It is preferable to make them even.
  • the holding time at each gas pressure stage in the range where the ratio of the gas flow rate is 1/5 to 1/2 is set (the wet filter Z and the dry filter) in the range where the ratio is 1/5 to 1/2. It is preferable that the average gas pressure holding time in the entire gas pressure stage be within 10% of soil.
  • the pressure increase value from one gas pressure stage to the next gas pressure stage is larger than the Sarian differential pressure when the fluid to be filtered is permeated at the linear velocity (J) in practical use. Closer is preferred.
  • the pressure is 1 to 10 times the transmembrane pressure. If the pressure increase value is too small, the gas-liquid interface does not move within the holding time, and if it is too large, the resolution of the pore diameter is lost. When there is a range in the transmembrane pressure, it is preferable that the transmembrane pressure is larger than the maximum transmembrane pressure.
  • the pressure increase value is controlled as described above at the gas pressure stage in the range where the gas flow rate ratio is 1/5 to 1/2, and further at all gas pressure stages in this range. Is preferred.
  • the respective boosted values should be as evenly as possible. Is preferred.
  • each boosted value in this range be within ⁇ 20% of the average boosted value in all gas pressure stages in this range.
  • the range in which the pressure holding time and the pressure increase width are managed is preferably from a lower pressure stage when the pore size distribution is wide.
  • the pressure increase value with respect to the previous gas pressure stage in each gas pressure stage, and each gas pressure holding time in each gas pressure stage are as described above, accurate and high accuracy can be obtained, An evaluation reflecting actual performance can be performed, but the average pore diameter is 0.05 to 2 microns, the thickness is 10 to 300 microns, If the flow rate of the filtration fluid is 11 O mZ days, and if the filter body is made of ceramics, considering the performance of the measuring device, the pressure increase value of each gas pressure step with respect to the previous gas pressure step is set to 0.01.
  • the gas pressure holding time in each gas pressure step can be selected from the range of 1 second to 1 minute. When measuring the dry filter, the pressure increase should be longer than the operation time of the device and the holding time longer than the response time. Good.
  • the pressurized gas used in the present invention is preferably, for example, an inert gas such as air, argon, or nitrogen, and is difficult to dissolve in a test liquid, taking into account evaluation conditions, detection means, cost, and the like. What is necessary is just to select suitably.
  • the permeated gas flow rate of each filter body is detected at each gas pressure stage, and the average pore diameter is determined based on equation (1).
  • the gas flow rate detected increases almost in proportion to the pressure increase of the pressurized gas because there is no pressurized gas in the pores. Medium and solid lines).
  • the test fluid to be pressed by the pressurized gas is present in the pores, and until the pressure of the pressurized gas overcomes the resistive force due to the surface tension of the test liquid, the gas is released.
  • One-liquid interface does not move.
  • the flow rate of the permeated gas starts to increase,
  • the gas flow overlaps with the permeated gas flow rate-gas pressure line in the dry filter (shown by the dotted line in the figure).
  • the permeated gas flow rate detected at each gas pressure from the time when the permeated gas flow rate starts to increase to the time when the permeated gas flow rate in the dry filter finally overlaps with the straight line of the gas pressure is determined by a series of gas passages. It changes depending on the pore size distribution of the pores.
  • the gas pressure H at which the flow rate of the permeated gas in the wet filter is 1 to 2 with respect to the flow rate of the permeate gas in the dry filter is determined. / 2), and the pore diameter corresponding to the gas pressure H is defined as the average pore diameter based on the equation (1).
  • the filter body was evaluated using the following sample, test liquid, and fluid to be filtered.
  • test liquid dry filter
  • test liquid dry filter
  • pressurized air was supplied to the pressurized gas supply side.
  • the pressure was increased by 0.017-0.02 IMP a every 30 seconds, and the gas flow rate was measured.
  • the sample was immersed in the test liquid, and the pores in the sample were completely filled with the test liquid.
  • a sample (wet filter) completely filled with the test liquid was placed in a holder of a pore diameter evaluation apparatus with its ends similarly sealed.
  • pressurized air was supplied to the pressurized gas supply side.
  • the gas pressure was maintained at each gas pressure level for 1 second, 2 seconds, 4 to 16 seconds, 9 to 11 seconds, 18 to 22 seconds, 25 to 30 seconds
  • the gas pressure was maintained at each gas pressure stage for 55-65 seconds, 290-310 seconds, 470-490 seconds, 590-610 seconds, and 0.017-0.02 IMP a each.
  • the pressure was increased and the gas flow was measured. From the gas pressure at which the gas flow rate of the wet filter was equal to the gas flow rate of the dry filter, the average pore diameter of each sample was determined based on equation (1).
  • the shorter the retention time the smaller the measurement result of the average pore diameter. If the retention time is longer than S, even if the connection path of the pore through which a part of the fluid to be filtered permeates in practical use is long, the gas permeates through the path even in a wet filter, and is evaluated. If the retention time is closer to S, an excessively long path through which the gas that permeates the dry filter and the part of the fluid to be filtered in practical use cannot permeate is less likely to be included in the evaluation, resulting in an accurate evaluation. . (Examples 7-28, Comparative Examples 5-26)
  • Example 16 The average pore diameter of 22 different samples was determined assuming that the gas pressure holding time in the gas permeation measurement of the wet filter of Example 16 was 911 seconds, and this was set as Example 7-28.
  • the average pore diameter was in the range of 0.13 to 0.15 ⁇ 1 (standard deviation 007).
  • Comparative Example 6-27 in which the gas pressure is maintained until the so-called gas saturation state is reached, and then the pressure is increased, the holding time at each gas pressure stage varies from 30 seconds to 20 minutes, and the average pore diameter Varied from 0.16 to 0.21 m (standard deviation: 0.011), and the average pore diameter was larger than the retention time of about 10 minutes shown in Fig. 4.
  • the present invention it is possible to accurately and accurately evaluate the average pore diameter of a filter having three-dimensionally intricate pores, and furthermore, to perform filtration during actual use. It is possible to provide a method for evaluating a filtration body capable of quality evaluation reflecting the performance of the body.

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un procédé de mesure de la taille des pores d'un matériau filtrant poreux qui reçoit un gaz sous pression administré à un matériau filtre sec et à un matériau filtre humide. Les pores sont remplis d'un liquide d'essai. La pression du gaz est augmentée par échelons, le taux d'écoulement du gaz introduit en perméation dans chaque matériau filtrant est décelé à chaque échelon de pression, puis la taille moyenne des pores est déterminée d'après l'expression mathématique (MFPD=(4BηCOSυ)/P).On augmente la pression pour l'échelon de pression suivant après avoir maintenu le matériau filtre humide sous une pression constante pendant (S)-30 secondes, lorsque le temps de passage (S) d'un filtrat déterminé selon l'expression mathématique (S=(X/J)xVs/Vr) est inférieur à 3 sec, ou pendant (S)-(Sx10) secondes si le temps de passage (S) du filtrat est supérieur ou égal à 3 secondes, sachant que X est l'épaisseur (m) du matériau filtrant, J est la vitesse de ligne (m/s) du filtrat en utilisation effective, Vs est la viscosité (Pas) du liquide d'essai et Vr est la viscosité (Pas) du filtrat. On peut ainsi mesurer la taille moyenne des pores avec une grande précision pour un matériau filtrant ayant des pores à structure tridimensionnelle complexe, et la qualité peut être évaluée par rapport à la performance du matériau filtrant à l'utilisation.
PCT/JP2004/003102 2003-03-24 2004-03-10 Procede de mesure de la taille des pores d'un materiau filtrant poreux WO2004086008A1 (fr)

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JP2003080107A JP3845067B2 (ja) 2003-03-24 2003-03-24 多孔質濾過体の細孔径測定方法

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101968430A (zh) * 2010-09-29 2011-02-09 西安航天华威化工生物工程有限公司 一种干法测量滤芯最大孔径的装置及方法
US8749783B2 (en) 2010-10-01 2014-06-10 Dow Global Technologies Llc System and method for analyzing pore sizes of substrates
CN111013395A (zh) * 2020-03-01 2020-04-17 贝士德仪器科技(北京)有限公司 滤膜前端控压方法及滤膜孔径测试装置
CN111678852A (zh) * 2020-05-11 2020-09-18 首钢集团有限公司 一种耐火材料气孔贯通性实验模具及方法

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JP4845004B2 (ja) * 2005-07-14 2011-12-28 財団法人電力中央研究所 細孔径分布測定方法
JP5811761B2 (ja) * 2011-10-18 2015-11-11 富士通株式会社 多孔質材料評価方法および多孔質材料評価装置
WO2018179959A1 (fr) 2017-03-30 2018-10-04 日本碍子株式会社 Procédé de test pour une structure de membrane de séparation, procédé de fabrication de module d'une membrane de séparation et procédé de fabrication d'une structure de membrane de séparation
KR101952432B1 (ko) * 2017-08-30 2019-02-26 주식회사 이덕아이앤씨 공극 지름 측정장치

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101968430A (zh) * 2010-09-29 2011-02-09 西安航天华威化工生物工程有限公司 一种干法测量滤芯最大孔径的装置及方法
US8749783B2 (en) 2010-10-01 2014-06-10 Dow Global Technologies Llc System and method for analyzing pore sizes of substrates
CN111013395A (zh) * 2020-03-01 2020-04-17 贝士德仪器科技(北京)有限公司 滤膜前端控压方法及滤膜孔径测试装置
CN111678852A (zh) * 2020-05-11 2020-09-18 首钢集团有限公司 一种耐火材料气孔贯通性实验模具及方法

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