WO2020085449A1 - Film microporeux de polyoléfine, filtre, support de chromatographie et bande pour immunochromatographie - Google Patents

Film microporeux de polyoléfine, filtre, support de chromatographie et bande pour immunochromatographie Download PDF

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WO2020085449A1
WO2020085449A1 PCT/JP2019/041768 JP2019041768W WO2020085449A1 WO 2020085449 A1 WO2020085449 A1 WO 2020085449A1 JP 2019041768 W JP2019041768 W JP 2019041768W WO 2020085449 A1 WO2020085449 A1 WO 2020085449A1
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polyolefin
polyolefin microporous
membrane
microporous membrane
film
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PCT/JP2019/041768
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English (en)
Japanese (ja)
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真実 南部
良和 幾田
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帝人株式会社
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Priority to KR1020217012026A priority Critical patent/KR102491301B1/ko
Priority to CN201980069817.5A priority patent/CN112912165B/zh
Publication of WO2020085449A1 publication Critical patent/WO2020085449A1/fr

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/26Polyalkenes
    • B01D71/261Polyethylene
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D63/00Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/005Microfluidic devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/26Polyalkenes
    • B01D71/262Polypropylene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • G01N33/544Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals the carrier being organic
    • G01N33/545Synthetic resin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2323/00Details relating to membrane preparation
    • B01D2323/02Hydrophilization
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/02Details relating to pores or porosity of the membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/04Characteristic thickness
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/20Specific permeability or cut-off range
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/36Hydrophilic membranes

Definitions

  • the present invention relates to a polyolefin microporous membrane, a filter, a chromatography carrier and an immunochromatographic strip.
  • Patent Document 1 the thickness is 1 to 350 ⁇ m, the porosity is 25 to 90%, the bubble point is 1 to 10 kg / cm 2 , the water permeation rate is 1000 liter / hr ⁇ m 2 ⁇ atm or more, and the surface water drop contact angle is 100.
  • a modified polyolefin porous membrane having a temperature of 0 ° or less is disclosed.
  • Patent Document 2 discloses a microporous polyolefin membrane having an average fibril diameter of 40 to 80 nm and an average pore diameter of 15 to 50 nm.
  • Patent Document 3 a water vapor permeation amount 4000 ⁇ 10000g / m 2 / 24hr , microporous polyolefin film is disclosed a water pressure resistance is at least 30 kPa.
  • the microporous polyolefin membrane may be used as a filter, a chromatography carrier, etc. for the purpose of separating, purifying or detecting substances.
  • a polyolefin microporous membrane having a small difference in porous structure between the surface direction and the thickness direction and having excellent isotropic mass transfer.
  • An embodiment of the present disclosure aims to provide a polyolefin microporous film having excellent isotropic mass transfer, and an object thereof is to solve the problem.
  • Formula (1) 0.7 ⁇ ⁇ X / ⁇ Z ⁇ 1.5
  • Formula (2) 0.7 ⁇ ⁇ Y / ⁇ Z ⁇ 1.5
  • ⁇ X Curvature ratio in the first direction along the first surface of the polyolefin microporous membrane.
  • ⁇ Y Curvature along a first surface of the polyolefin microporous membrane and in a second direction orthogonal to the first direction.
  • ⁇ Z Curvature ratio in the thickness direction of the polyolefin microporous film.
  • T X Permeability index in the first direction along the first surface of the microporous polyolefin membrane.
  • T Y Permeability index in the second direction along the first surface of the polyolefin microporous membrane and orthogonal to the first direction.
  • TZ Permeability index in the thickness direction of the polyolefin microporous membrane.
  • the hydrophilic polyolefin microporous membrane is a polyolefin microporous membrane in which at least one of the membrane surface and the pore inner surface is physically hydrophilized, [7] or [8] Polyolefin microporous membrane.
  • a polyolefin microporous membrane having excellent isotropic mass transfer is provided.
  • 3 is a cross-sectional image obtained by X-ray CT of the microporous polyolefin membrane of Example 1.
  • 3 is a cross-sectional image obtained by X-ray CT of the microporous polyolefin membrane of Example 2.
  • 5 is a cross-sectional image obtained by X-ray CT of the microporous polyolefin membrane of Example 3.
  • 4 is a cross-sectional image obtained by X-ray CT of the microporous polyolefin membrane of Comparative Example 1.
  • 5 is a cross-sectional image obtained by X-ray CT of the microporous polyolefin membrane of Comparative Example 2.
  • 3 is a graph showing changes in absorbance with time in Example 2 and Comparative Example 1.
  • the numerical range indicated by using “to” indicates the range including the numerical values before and after “to” as the lower limit value and the upper limit value, respectively.
  • the upper limit or the lower limit described in one numerical range may be replaced with the upper limit or the lower limit of the numerical range described in other stages.
  • the upper limit value or the lower limit value of the numerical range may be replaced with the value shown in the examples.
  • process is included in this term as long as the intended purpose of the process is achieved, not only when it is an independent process but also when it cannot be clearly distinguished from other processes.
  • each component may include multiple types of applicable substances.
  • the amount of each component in the composition when referring to the amount of each component in the composition, when a plurality of substances corresponding to each component are present in the composition, the plurality of substances present in the composition are included unless otherwise specified. Means the total amount of a substance.
  • machine direction means a long direction in a film, film or sheet manufactured in a long shape
  • width direction means a direction orthogonal to the “machine direction”.
  • machine direction is also referred to as “MD direction”
  • TD direction width direction
  • the present disclosure provides a polyolefin microporous membrane having excellent isotropic mass transfer.
  • a polyolefin microporous film means that a fibrillar polyolefin forms a three-dimensional network structure, has a large number of fine pores inside, and has a structure in which these fine pores are connected. It means a membrane that allows gas or liquid to pass to the other surface.
  • the present disclosure discloses a first polyolefin microporous membrane and a second polyolefin microporous membrane as a polyolefin microporous membrane having excellent isotropic mass transfer.
  • the first polyolefin microporous film has a film thickness of 1 ⁇ m to 400 ⁇ m and satisfies the following formulas (1) and (2).
  • Formula (1) 0.7 ⁇ ⁇ X / ⁇ Z ⁇ 1.5
  • Formula (2) 0.7 ⁇ ⁇ Y / ⁇ Z ⁇ 1.5
  • ⁇ X Curvature ratio in the first direction along the first surface of the polyolefin microporous membrane.
  • ⁇ Y Curvature along a first surface of the polyolefin microporous membrane and in a second direction orthogonal to the first direction.
  • ⁇ Z Curvature ratio in the thickness direction of the polyolefin microporous film.
  • the first surface of the polyolefin microporous film means one of two main surfaces of the polyolefin microporous film (for example, when one surface is defined as a surface, the front surface and the back surface correspond to the two main surfaces). Point to.
  • the direction along the first surface of the polyolefin microporous membrane is orthogonal to the thickness direction of the polyolefin microporous membrane. Therefore, the first direction, the second direction, and the thickness direction are orthogonal to each other.
  • the tortuosity is an index indicating how much the flow path through which the fluid flows detours with respect to the shortest distance, and the detouring of the flow path increases the tortuosity.
  • the first microporous polyolefin membrane is excellent in mass transfer isotropy by simultaneously satisfying the formulas (1) and (2).
  • ⁇ X / ⁇ Z or ⁇ Y / ⁇ Z is less than 0.7 in the microporous polyolefin membrane, the degree of bypass of the flow path is too large in the thickness direction, and the fluid is hard to spread in the thickness direction.
  • ⁇ X / ⁇ Z or ⁇ Y / ⁇ Z is more than 1.5 in the polyolefin microporous film, the degree of bypass of the flow path is too large in the plane direction, and the fluid is hard to spread in the plane direction.
  • the first microporous polyolefin membrane preferably satisfies the formula (1 ′): 0.75 ⁇ ⁇ X / ⁇ Z ⁇ 1.3 from the viewpoint of more excellent isotropic mass transfer, and the formula (1 ′) '): It is more preferable to satisfy 0.8 ⁇ ⁇ X / ⁇ Z ⁇ 1.1.
  • the first microporous polyolefin membrane preferably satisfies the formula (2 ′): 0.75 ⁇ ⁇ Y / ⁇ Z ⁇ 1.3 from the viewpoint of being more excellent in isotropic mass transfer, and the formula (2 ′) '): It is more preferable to satisfy 0.8 ⁇ ⁇ Y / ⁇ Z ⁇ 1.1.
  • the first microporous polyolefin membrane preferably satisfies the formulas (1) and (2 ′) at the same time, and more preferably satisfies the formulas (1) and (2 ′′) at the same time.
  • the first polyolefin microporous membrane preferably satisfies the formula (1 ′) and the formula (2) at the same time, more preferably satisfies the formula (1 ′) and the formula (2 ′) at the same time, and the formula (1 It is more preferable to satisfy both ') and formula (2'') at the same time.
  • the first polyolefin microporous membrane preferably satisfies the formula (1 ′′) and the formula (2) at the same time, and more preferably satisfies the formula (1 ′′) and the formula (2 ′) at the same time. It is more preferable to satisfy both (1 '') and formula (2 '') at the same time.
  • ⁇ X is not particularly limited, but is preferably 1.2 to 2.0, more preferably 1.2 to 1.8, and further preferably 1.4 to 1.7.
  • ⁇ Y is not particularly limited, but is preferably 1.2 to 2.0, more preferably 1.2 to 1.8, and further preferably 1.4 to 1.7.
  • ⁇ Z is not particularly limited, but is preferably 1.3 to 2.1, more preferably 1.5 to 2.0, still more preferably 1.6 to 1.9.
  • the second polyolefin microporous film has a film thickness of 1 ⁇ m to 400 ⁇ m and satisfies the following formulas (3) and (4).
  • T X Permeability index in the first direction along the first surface of the microporous polyolefin membrane.
  • T Y Permeability index in the second direction along the first surface of the polyolefin microporous membrane and orthogonal to the first direction.
  • TZ Permeability index in the thickness direction of the polyolefin microporous membrane.
  • the first surface of the polyolefin microporous film means one of two main surfaces of the polyolefin microporous film (for example, when one surface is defined as a surface, the front surface and the back surface correspond to the two main surfaces). Point to.
  • the direction along the first surface of the polyolefin microporous membrane is orthogonal to the thickness direction of the polyolefin microporous membrane. Therefore, the first direction, the second direction, and the thickness direction are orthogonal to each other.
  • the permeability index (Permeability) is an index indicating the ease of flow of a fluid in a flow path of the fluid, and the permeability index is larger as the flow path of the fluid is easier.
  • the permeability index is a wet area derived from the Darcy-Weissbach equation, and has a unit of length squared ( ⁇ m 2 ).
  • the second polyolefin microporous membrane is excellent in mass transfer isotropy by simultaneously satisfying the expressions (3) and (4).
  • T X / T Z or T Y / T Z is less than 0.5 in the polyolefin microporous film, the fluid flows too much in the thickness direction as compared with the plane direction, and the fluid is less likely to spread in the plane direction.
  • T X / T Z or T Y / T Z is more than 2.0 in the microporous polyolefin membrane, the fluid flows too much in the surface direction as compared with the thickness direction, and it is difficult for the fluid to spread in the thickness direction.
  • the second polyolefin microporous membrane preferably satisfies the formula (3 ′): 0.8 ⁇ T X / T Z ⁇ 2.0, from the viewpoint of being superior in isotropic mass transfer, and the formula (3 ′) '): It is more preferable to satisfy 0.9 ⁇ T X / T Z ⁇ 1.9.
  • the second microporous polyolefin membrane preferably satisfies the formula (4 ′): 0.75 ⁇ T Y / T Z ⁇ 1.5 from the viewpoint of being more excellent in the mass transfer isotropy, and the formula (4 ′) '): It is more preferable to satisfy 0.8 ⁇ T Y / T Z ⁇ 1.1.
  • the second polyolefin microporous film preferably satisfies the formulas (3) and (4 ′) at the same time, and more preferably satisfies the formulas (3) and (4 ′′) at the same time.
  • the second polyolefin microporous membrane preferably satisfies the formula (3 ′) and the formula (4) at the same time, more preferably satisfies the formula (3 ′) and the formula (4 ′) at the same time, and the formula (3 It is more preferable to satisfy both ') and equation (4'') at the same time.
  • the second polyolefin microporous membrane preferably satisfies the formula (3 ′′) and the formula (4) at the same time, and more preferably satisfies the formula (3 ′′) and the formula (4 ′) at the same time. It is more preferable to satisfy both (3 ′′) and equation (4 ′′) at the same time.
  • T X is not particularly limited, it is preferably 0.4 to 3.0, more preferably 0.5 to 2.5, and further preferably 1.0 to 2.0.
  • T Y is not particularly limited, it is preferably 0.2 to 2.0, more preferably 0.3 to 1.9, still more preferably 0.5 to 1.8.
  • T Z is not particularly limited, it is preferably 0.2 to 2.0, more preferably 0.3 to 1.9, still more preferably 0.5 to 1.8.
  • the polyolefin microporous film is subjected to X-ray computed tomography (X-ray CT), the sample is taken an X-ray transmission image while rotating it by 0 ° to 180 °, and a three-dimensional image of the internal structure is computerized from the obtained image data. Rebuild with. The reconstructed three-dimensional image is subjected to image conversion by image processing software ImageJ, and cross-sectional sequence data of 0.26 ⁇ m / pixel pitch is obtained for each of three planes (XY plane, XZ plane, YZ plane).
  • X-ray CT X-ray computed tomography
  • ImageJ image processing software
  • the axial direction of the sequence data is set to the image processing software ImageJ so that the Z direction of the three views may coincide with the thickness direction of the polyolefin microporous film. Convert with. If necessary, the image processing software ImageJ is used to create a three-view drawing.
  • the X direction and the Y direction in the three-view drawing are not particularly limited, but are, for example, the MD direction and the TD direction or the TD direction and the MD direction of the polyolefin microporous film, respectively.
  • a network is constructed by connecting the centers of the nearest voids in order in the X direction, the Y direction, and the Z direction, respectively, and determining the contact area between the closest voids. Get as a parameter. Then, a simulation is performed in which the fluid is caused to flow in a constant amount of outflow water in each of the X direction, the Y direction, and the Z direction, and the complexity and permeability of the network are analyzed.
  • the length of the fluid flow direction is the length of the flow path, and the area of the plane orthogonal to the fluid flow direction is the cross-sectional area.
  • the simulation conditions are: fluid viscosity: 0.001 Pa ⁇ s, inlet pressure: 130 MPa, outlet pressure: 100 MPa, and the pressure difference between the inlet and the outlet is 30 MPa.
  • ⁇ X , ⁇ Y, and ⁇ Z which are the turn rates in the X direction, the Y direction, and the Z direction
  • T X , T which are the transmission indices in the X direction, the Y direction, and the Z direction, respectively.
  • the tortuosity ratio is the average value of the values obtained by dividing the length of the network connecting one surface to the other surface by the shortest distance connecting the start point and the end point of the network.
  • the permeability index is a coefficient derived from the Darcy-Weissbach equation. In the Darcy-Weissbach equation, substitute the outflow water amount per unit time for Q, the viscosity of the fluid for ⁇ , the flow path length for L, the pressure difference for ⁇ P, and the cross-sectional area for A. Find k.
  • the first polyolefin microporous membrane and the second polyolefin microporous membrane will be described in more detail. Items common to the first polyolefin microporous membrane and the second polyolefin microporous membrane will be collectively described as the polyolefin microporous membrane of the present disclosure.
  • the polyolefin microporous membrane of the present disclosure may be hydrophobic or hydrophilic. Since polyolefin is a hydrophobic resin, the microporous polyolefin membrane itself is hydrophobic.
  • the polyolefin microporous membrane of the present disclosure may be a hydrophobic polyolefin microporous membrane that is not subjected to a hydrophilizing treatment, or may be a polyolefin microporous membrane that is rendered hydrophilic by the hydrophilizing treatment. Details of the method for hydrophilizing the polyolefin microporous membrane will be described later.
  • the fact that the polyolefin microporous membrane is hydrophilic means that the contact angle of water after dropping 1 second is 90 degrees or less on at least one surface.
  • the contact angle of water 1 second after dropping is a value measured by the measuring method described later.
  • polyolefin microporous membrane of the present disclosure other than the bend ratio and the permeability index will be described.
  • the characteristics common to the hydrophobic polyolefin microporous membrane and the hydrophilic polyolefin microporous membrane will be simply described as “polyolefin microporous membrane” and the characteristics will be described.
  • the film thickness of the polyolefin microporous film of the present disclosure is appropriately 1 ⁇ m to 400 ⁇ m, and may be selected within the range according to the application, for example, 10 ⁇ m to 300 ⁇ m, 20 ⁇ m to 250 ⁇ m, 30 ⁇ m to 200 ⁇ m. And 40 ⁇ m to 150 ⁇ m.
  • the bubble point pressure of the polyolefin microporous membrane of the present disclosure may be selected according to the application, and is, for example, 0.001 MPa or more and less than 0.1 MPa, 0.005 MPa to 0.08 MPa, 0.007 MPa to 0. It is 0.05 MPa.
  • the bubble point pressure of the polyolefin microporous membrane is obtained by immersing the polyolefin microporous membrane in ethanol and following the bubble point test method of JIS K3832: 1990, except that the liquid temperature during the test is changed to 24 ⁇ 2 ° C. It is a value obtained by performing a bubble point test while increasing the applied pressure at a pressure increasing rate of 2 kPa / sec.
  • the ethanol flow rate of the polyolefin microporous membrane of the present disclosure may be selected depending on the application.
  • the value obtained by multiplying the ethanol flow rate (mL / (min ⁇ cm 2 ⁇ MPa)) and the film thickness ( ⁇ m) is, for example, 50,000 to 500,000, and 80,000 to 40,000. It is 100,000 to 300,000.
  • the flow rate of ethanol (mL / (min ⁇ cm 2 ⁇ MPa)) of the polyolefin microporous membrane is the same as that of the polyolefin microporous membrane set in the liquid permeation cell having a constant liquid permeation area (cm 2 ).
  • 100 mL of ethanol is permeated at (kPa), and the time (sec) required for 100 mL of ethanol to permeate is measured and converted into units.
  • Gurley value The Gurley value (second / 100 mL ⁇ ⁇ m) per unit thickness of the polyolefin microporous membrane of the present disclosure may be selected according to the application, and is, for example, 0.0005 to 0.1, 0.005 to 0. 0.05 and 0.01 to 0.03.
  • the Gurley value of the polyolefin microporous film is a value measured according to JIS P8117: 2009.
  • the porosity of the polyolefin microporous membrane of the present disclosure may be selected according to the application, and is, for example, 70% to 95%, 75% to 93%, 80% to 92%.
  • the constituent materials of the microporous polyolefin membrane are a, b, c, ..., N, and the masses of the constituent materials are Wa, Wb, Wc, ..., Wn (g / cm 2 ), respectively.
  • the true density of the material is xa, xb, xc, ..., Xn (g / cm 3 ), and the film thickness of the polyolefin microporous film is t (cm).
  • the average flow pore size of the polyolefin microporous membrane of the present disclosure may be selected according to the application, and is, for example, 0.02 ⁇ m to 5 ⁇ m, 0.05 ⁇ m to 4 ⁇ m, or 0.1 ⁇ m to 3.5 ⁇ m.
  • the average flow pore size of the polyolefin microporous membrane was measured by using a Palm Porometer (model: CFP-1200-AEXL) manufactured by PMI, and using a Glwick (surface tension 15.9 dyn / cm) manufactured by PMI as the immersion liquid. Obtained based on the half-dry method specified in ASTM E1294-89.
  • the BET specific surface area of the polyolefin microporous membrane of the present disclosure may be selected according to the application, and is, for example, 1 m 2 / g to 30 m 2 / g, 2 m 2 / g to 25 m 2 / g, or 3 m 2. / G to 20 m 2 / g.
  • the BET specific surface area of the polyolefin microporous membrane is set by a nitrogen gas adsorption method under liquid nitrogen temperature using a specific surface area measuring device (model: BELSORP-mini) manufactured by Microtrac Bell Co., Ltd .: relative pressure set to 1.0. It is a value obtained by measuring an adsorption isotherm of ⁇ 10 ⁇ 3 to 0.35 and analyzing it by the BET method.
  • the puncture strength per unit thickness of the polyolefin microporous membrane of the present disclosure is, for example, 0.05 g / ⁇ m to 1.5 g / ⁇ m, 0.07 g / ⁇ m to 1.2 g / ⁇ m, and 0. It is from 08 g / ⁇ m to 1.0 g / ⁇ m.
  • the puncture strength per unit thickness of the polyolefin microporous membrane is the maximum puncture load (g) measured by performing a needle penetration test (needle: radius of curvature of tip: 0.5 mm, puncture speed: 320 mm / min). It is determined by dividing the load by the film thickness ( ⁇ m) of the polyolefin microporous film.
  • the contact angle of water after dropping for 1 second on at least one surface is 0 to 90 degrees.
  • the contact angle of water on both sides after dropping 1 second is 0 to 90 degrees.
  • the contact angle of water on the surface of the hydrophilic polyolefin microporous membrane after 1 second of dropping may be selected according to the application, for example, 1 degree to 80 degrees, 3 degrees to 70 degrees, and 5 degrees to It is 60 degrees.
  • the contact angle of water 1 second after dropping is a value measured by the following measuring method.
  • 1 ⁇ L of a water drop was dropped on the surface of the polyolefin microporous film by a syringe, and the static contact angle of water 1 second after the dropping was ⁇ by using a fully automatic contact angle meter. / 2 method.
  • the polyolefin contained in the polyolefin microporous membrane of the present disclosure is not particularly limited, and examples thereof include polyethylene, polypropylene, polybutylene, polymethylpentene, and a copolymer of polypropylene and polyethylene.
  • polyethylene is preferable, and high density polyethylene, a mixture of high density polyethylene and ultra high molecular weight polyethylene, and the like are suitable.
  • the polyolefin microporous membrane a polyethylene microporous membrane in which the contained polyolefin is only polyethylene is suitable.
  • the polyolefin microporous membrane of the present disclosure includes a polyolefin composition (in the present disclosure, means a mixture of polyolefins containing two or more kinds of polyolefins, and when the contained polyolefin is only polyethylene, it is referred to as a polyethylene composition). Is preferred.
  • the polyolefin composition forms a network structure with fibrillation during stretching, and has the effect of increasing the porosity of the microporous polyolefin membrane.
  • the polyolefin composition is preferably a polyolefin composition containing 3% by mass to 15% by mass of ultrahigh molecular weight polyethylene having a weight average molecular weight of 9 ⁇ 10 5 or more with respect to the total amount of the polyolefin, and 5% by mass to 10% by mass. %, A polyolefin composition containing 5% by mass to 8% by mass is more preferable.
  • the polyolefin composition comprises an ultra high molecular weight polyethylene having a weight average molecular weight of 9 ⁇ 10 5 or more, a weight average molecular weight of 2 ⁇ 10 5 to 8 ⁇ 10 5 , and a density of 0.92 g / cm 3 to 0.96 g / cm.
  • the high density polyethylene of 3 is a polyolefin composition mixed in a mass ratio of 3:97 to 15:85 (more preferably 5:95 to 10:90, further preferably 5:95 to 8:92). Is preferred.
  • the weight average molecular weight of the entire polyolefin is preferably 2 ⁇ 10 5 to 2 ⁇ 10 6 .
  • the weight average molecular weight of the polyolefin constituting the polyolefin microporous membrane of the present disclosure is determined by dissolving the polyolefin microporous membrane in o-dichlorobenzene by heating and performing gel permeation chromatography (system: Waters company Alliance GPC 2000 type, column: GMH6. -HT and GMH6-HTL), the column temperature is 135 ° C. and the flow rate is 1.0 mL / min.
  • Molecular weight monodisperse polystyrene manufactured by Tosoh Corporation is used to calibrate the molecular weight.
  • the polyolefin microporous membrane of the present disclosure can be produced, for example, by a production method including the following steps (I) to (IV).
  • Step (I) is a step of preparing a solution containing the polyolefin composition and a volatile solvent having a boiling point of less than 210 ° C. at atmospheric pressure.
  • the solution is preferably a thermoreversible sol-gel solution, and the polyolefin composition is heated and dissolved in a solvent to form a sol, thereby preparing a thermoreversible sol-gel solution.
  • the volatile solvent having a boiling point of less than 210 ° C. at atmospheric pressure is not particularly limited as long as it is a solvent capable of sufficiently dissolving polyolefin.
  • volatile solvent examples include tetralin (206 ° C to 208 ° C), ethylene glycol (197.3 ° C), decalin (decahydronaphthalene, 187 ° C to 196 ° C), toluene (110.6 ° C), xylene. (138 ° C. to 144 ° C.), diethyltriamine (107 ° C.), ethylenediamine (116 ° C.), dimethylsulfoxide (189 ° C.), hexane (69 ° C.), and the like, with decalin or xylene being preferred (the temperature in parentheses is Boiling point at atmospheric pressure.).
  • the volatile solvents may be used alone or in combination of two or more kinds.
  • the polyolefin composition used in the step (I) (in the present disclosure, means a mixture of polyolefins containing two or more kinds of polyolefins, and when the contained polyolefin is only polyethylene, it is referred to as a polyethylene composition) contains polyethylene.
  • a polyethylene composition is more preferable, and a polyethylene composition is more preferable.
  • the solution prepared in step (I) preferably has a concentration of the polyolefin composition of 10% by mass to 40% by mass, and 15% by mass. It is more preferably from about 35% by mass.
  • concentration of the polyolefin composition is 10% by mass or more, the occurrence of cutting can be suppressed in the process of forming the polyolefin microporous film, and the mechanical strength of the polyolefin microporous film is increased to improve the handling property.
  • the concentration of the polyolefin composition is 40% by mass or less, pores of the polyolefin microporous film are likely to be formed.
  • Step (II) is a step of melt-kneading the solution prepared in step (I), extruding the obtained melt-kneaded product through a die, and cooling and solidifying to obtain a first gel-like molded product.
  • an extrudate is obtained by extruding from a die in a temperature range of melting point to melting point + 65 ° C of the polyolefin composition, and then the extrudate is cooled to obtain a first gel-like molded product.
  • the first gel-like molded product is preferably shaped into a sheet. Cooling may be carried out by immersion in water or an organic solvent, or contact with a cooled metal roll, generally by immersion in the volatile solvent used in step (I). Done.
  • Step (III) is a step of stretching the first gel-like molded product in at least one direction (primary stretching) and drying the solvent to obtain a second gel-like molded product.
  • the stretching step of step (III) is preferably biaxial stretching, and may be sequential biaxial stretching in which longitudinal stretching and transverse stretching are carried out separately, or simultaneous biaxial stretching in which longitudinal stretching and transverse stretching are carried out simultaneously.
  • the stretching ratio of the primary stretching (the product of the longitudinal stretching ratio and the lateral stretching ratio) is preferably 1.1 to 3 times from the viewpoint of controlling the isotropicity of the porous structure of the polyolefin microporous membrane, and the temperature during stretching Is preferably 75 ° C. or lower.
  • the drying step of step (III) is carried out without particular limitation as long as it is a temperature at which the second gel-like molded product is not deformed, but it is preferably carried out at 60 ° C or lower.
  • the stretching step and the drying step of the step (III) may be performed simultaneously or stepwise.
  • primary stretching may be performed while preliminary drying is performed, and then main drying may be performed, or primary stretching may be performed between preliminary drying and main drying.
  • the primary stretching can be performed in a state where the drying is controlled and the solvent remains in a suitable state.
  • Step (IV) is a step of stretching (secondarily stretching) the second gel-like molded product in at least one direction.
  • the stretching step of step (IV) is preferably biaxial stretching.
  • the stretching step of step (IV) includes sequential biaxial stretching in which longitudinal stretching and transverse stretching are separately performed; simultaneous biaxial stretching in which longitudinal stretching and transverse stretching are simultaneously performed; transverse stretching after multiple stretching in the longitudinal direction. Stretching step in the longitudinal direction and plural times in the transverse direction; sequential biaxial stretching and then further stretching in the longitudinal direction and / or the transverse direction once or plural times.
  • the stretching ratio of the secondary stretching is preferably 2 to 25 times, more preferably from the viewpoint of controlling the isotropicity of the porous structure of the polyolefin microporous membrane. It is 5 to 20 times, more preferably 8 to 15 times.
  • the stretching temperature of the secondary stretching is preferably 90 ° C. to 135 ° C., and more preferably 90 ° C. to 125 ° C. from the viewpoint of controlling the isotropicity of the porous structure of the polyolefin microporous film.
  • Heat fixing may be performed after step (IV).
  • the heat setting temperature is preferably 120 ° C. to 150 ° C., and more preferably 125 ° C. to 140 ° C., from the viewpoint of controlling the isotropy of the porous structure of the polyolefin microporous membrane.
  • the solvent remaining in the microporous polyolefin membrane may be subjected to an extraction treatment and an annealing treatment.
  • the extraction treatment of the residual solvent is performed, for example, by immersing the sheet after the heat fixing treatment in a methylene chloride bath to elute the residual solvent in methylene chloride.
  • the polyolefin microporous membrane immersed in the methylene chloride bath is preferably removed from the methylene chloride bath by drying after removing the methylene chloride bath.
  • the annealing treatment is performed by transporting the polyolefin microporous film on a roller heated to, for example, 100 ° C. to 140 ° C. after the residual solvent is extracted.
  • the stretching ratio (product of the longitudinal stretching ratio and the transverse stretching ratio) of the secondary stretching is 2 to 25 times. It can be listed in the range of.
  • the stretching ratio of the secondary stretching is 2 to 25 times. It can be listed in the range of. The larger the mass ratio of the ultrahigh molecular weight polyethylene contained in the polyolefin composition, the smaller the values of T X , T Y and T Z tend to be.
  • Examples of the treatment method for making the hydrophobic polyolefin microporous membrane hydrophilic include, for example, a method of applying a hydrophilic material to at least one of the membrane surface and the pore inner surface of the hydrophobic polyolefin microporous membrane, or the hydrophobic polyolefin microporous membrane. There may be mentioned a method in which at least one of the surface of the film and the inner surface of the pores is physically hydrophilized.
  • Specific examples of the method for applying a hydrophilic material to at least one of the membrane surface and the pore inner surface of the hydrophobic polyolefin microporous membrane include, for example, coating with a surfactant or a hydrophilic material, graft polymerization of a hydrophilic monomer. Is mentioned.
  • the surfactant that hydrophilizes the hydrophobic polyolefin microporous membrane may be any of a cationic surfactant, an anionic surfactant, a zwitterionic surfactant, and a nonionic surfactant.
  • a cationic surfactant include higher amine halogenate, alkylpyridinium halide, quaternary ammonium salt and the like.
  • anionic surfactant higher fatty acid alkali salt, polyoxyethylene alkyl ether sulfonate ester salt, polyoxyethylene alkyl ether phosphonate salt, alkyl sulfate salt, alkyl benzene sulfate salt, alkyl sulfonate salt, alkyl aryl sulfonate salt
  • examples thereof include salts and sulfosuccinic acid ester salts. Of these, alkylbenzene sulfonate is preferable, and sodium dodecylbenzene sulfonate is particularly preferable.
  • Examples of the zwitterionic surfactant include alkylbetaine compounds, imidazoline compounds, alkylamine oxides, bisoxyborate compounds and the like.
  • Examples of the nonionic surfactant include polyoxyethylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene alkyl allyl ethers, glycerin fatty acid ester, polyoxyethylene sorbitan fatty acid ester, and sorbitan fatty acid ester. .
  • hydrophilic materials for coating the hydrophobic polyolefin microporous membrane include cellulose, polyvinyl alcohol, polyethylene-polyvinyl alcohol copolymer, polyurethane, polyacrylamide and the like.
  • the polyolefin microporous membrane of the present disclosure is used, for example, for the purpose of separation, purification, concentration, fractionation, detection, etc. of a substance dispersed or dissolved in a fluid (that is, gas or liquid).
  • a fluid that is, gas or liquid.
  • the hydrophilic composite membrane of the present disclosure for example, gas-liquid separation, water purification, sterilization, seawater desalination, artificial dialysis, pharmaceutical production, food production, medical equipment, in-vitro diagnostic agents, filters used in in-vitro diagnostic equipment, etc. Chromatographic carrier; and the like.
  • Chromatographic carrier is the stationary phase of chromatography. Chromatography and chromatographic carriers are known, and any known form may be applied to construct a chromatographic carrier comprising the polyolefin microporous membrane of the present disclosure.
  • a more specific example of the form of the chromatography carrier containing the polyolefin microporous membrane of the present disclosure is a chromatography carrier contained in an immunochromatographic strip.
  • Examples of the form of the immunochromatographic strip to which the microporous polyolefin membrane of the present disclosure is applied include the following forms.
  • a polyolefin microporous membrane of the present disclosure A detection unit provided in the polyolefin microporous film, the detection unit fixed with a detection reagent that specifically binds to the substance to be detected, Immunochromatographic strip containing.
  • the polyolefin microporous membrane of the present disclosure functions as a chromatography carrier (stationary phase) in the immunochromatographic strip of the present disclosure.
  • the liquid sample moves through the chromatographic carrier (that is, the polyolefin microporous membrane of the present disclosure), and the substance to be detected contained in the liquid sample is concentrated in the detection portion and is visually observed. Alternatively, it is detected using a device.
  • a preferred embodiment of the immunochromatographic strip is A sample pad for receiving a liquid sample that may contain the substance to be detected, A conjugate pad containing a labeling substance that specifically binds to the substance to be detected, The polyolefin microporous membrane of the present disclosure to which a detection reagent that specifically binds to the substance to be detected is fixed.
  • FIG. 1 shows an embodiment of the immunochromatographic strip of the present disclosure.
  • the immunochromatographic strip A comprises a sample pad 2 for receiving a dropped sample, a conjugate pad 3 containing a labeling substance, and a detection reagent from upstream to downstream in the developing direction (direction shown by arrow X in FIG. 1).
  • the fixed chromatography carrier 1 and the absorption pad 4 for absorbing an excess sample are fixed in this order on a resin support 5.
  • the chromatography carrier 1 includes the polyolefin microporous membrane of the present disclosure and a detection unit 11 provided on the polyolefin microporous membrane.
  • the detection unit 11 is a region where a detection reagent that specifically binds to the substance to be detected is fixed.
  • the polyolefin microporous membrane of the present disclosure is preferably used as the chromatography carrier 1 after being lined with a film.
  • Chromatography carrier 1 includes the polyolefin microporous membrane of the present disclosure.
  • the TD direction of the polyolefin microporous membrane of the present disclosure and the developing direction of the sample match.
  • the MD direction of the polyolefin microporous membrane of the present disclosure and the sample developing direction match.
  • an example of the detection unit 11 is linearly formed in an arbitrary position of the polyolefin microporous film in a direction orthogonal to the developing direction.
  • the detection unit 11 may be formed in a circular spot, a number, a character, a symbol (for example, +, ⁇ ) or the like at an arbitrary position of the polyolefin microporous film.
  • the chromatography carrier 1 may further include, downstream of the detection unit 11, a control unit that is a region in which a control substance that specifically binds to the labeling substance is fixed.
  • a control unit downstream of the detection unit 11
  • the sample moves to the control unit after passing through the detection unit 11
  • a labeling substance that is not captured by the detection unit 11 that is, a substance to be detected is bound
  • Non-labeled substance specifically binds to the control substance, whereby the labeled substance is concentrated in the control part.
  • the immunochromatographic strip is known, and any known form may be applied to configure the immunochromatographic strip A.
  • the polyolefin microporous membrane of the present disclosure included in the immunochromatographic strip A is preferably a hydrophilic polyolefin microporous membrane.
  • the hydrophilic polyolefin microporous membrane of the present disclosure constitutes the immunochromatographic strip A, the surface of the hydrophilic polyolefin microporous membrane having a water contact angle of 0 to 90 degrees after 1 second of dropping is a substance to be detected.
  • the immunochromatographic strip of the present disclosure has excellent inspection accuracy.
  • the mechanism is speculated as follows.
  • the detection part is provided in a part of the chromatography carrier by applying a liquid composition containing the detection reagent to the chromatography carrier.
  • the liquid composition is more likely to flow in the surface direction than in the thickness direction, and as a result, the area of the detection section is expanded and the concentration of the detection reagent contained in the detection section is equal to the expected value. Will be lower than.
  • the liquid composition containing the detection reagent flows in the thickness direction to the same extent as the surface direction, so that the area of the detection unit is widened.
  • the concentration of the detection reagent contained in the detection unit becomes close to the expected value.
  • the concentration of the detection reagent is close to the expected value, and thus the immunochromatographic strip of the present disclosure is excellent in inspection accuracy.
  • the immunochromatographic strip of the present disclosure takes a short time to complete the test.
  • the mechanism is speculated as follows. Since the detection part is formed with a depth in the thickness direction of the chromatography carrier, in order to saturate the specific binding between the detection reagent contained in the detection part and the detection target substance, the detection target substance is It is necessary to reach the detection section over the entire thickness direction.
  • the mobile phase is more likely to flow in the surface direction than in the thickness direction, and since it takes time for the mobile phase to spread in the thickness direction, the substance to be detected is spread over the entire thickness direction. It takes time to reach the detector.
  • the conventional polyolefin microporous membrane it takes time for the specific binding between the detection reagent and the substance to be detected contained in the detection portion to be saturated, and the time required for completing the inspection becomes long.
  • the polyolefin microporous membrane of the present disclosure which is excellent in isotropic mass transfer, the mobile phase flows in the thickness direction to the same extent as the plane direction, so that the substance to be detected reaches the detection portion over the entire thickness direction. Time is reduced. Therefore, in the polyolefin microporous film of the present disclosure, the time required for saturating the specific bond between the detection reagent contained in the detection part and the substance to be detected is shortened, and the time required for completing the test is shortened.
  • polyolefin microporous membrane of the present disclosure will be described more specifically with reference to Examples. Materials, usage amounts, ratios, processing procedures, and the like shown in the following examples can be appropriately changed without departing from the spirit of the present disclosure. Therefore, the scope of the polyolefin microporous membrane of the present disclosure should not be limitedly construed by the specific examples shown below.
  • Example 1 2.5 parts by weight of ultra-high molecular weight polyethylene (hereinafter referred to as “UHMWPE”) having a weight average molecular weight of 4.6 million, and high density polyethylene (hereinafter referred to as “HDPE”) having a weight average molecular weight of 560,000 and a density of 950 kg / m 3 .
  • UHMWPE ultra-high molecular weight polyethylene
  • HDPE high density polyethylene
  • a polyethylene composition mixed with 5 parts by mass was prepared.
  • a polyethylene solution was prepared by mixing the polyethylene composition and decalin so that the polymer concentration was 25% by mass.
  • the above polyethylene solution was extruded into a sheet form from a die at a temperature of 147 ° C., and then the extrudate was cooled in a water bath having a water temperature of 20 ° C. to obtain a first gel-like sheet.
  • the first gel-like sheet is pre-dried in a temperature atmosphere of 70 ° C. for 10 minutes, then primary stretched 1.1 times in the MD direction, and then the main drying is performed in a temperature atmosphere of 57 ° C. for 5 minutes.
  • the operation was performed for a minute to obtain a second gel-like sheet (base tape) (the residual amount of the solvent in the second gel-like sheet was less than 1%).
  • the second gel-like sheet (base tape) is stretched in the MD direction at a temperature of 90 ° C. at a draw ratio of 2 times, and then in the TD direction at a temperature of 130 ° C. at a draw ratio of 5 times, and Immediately, heat treatment (heat setting) was performed at 140 ° C.
  • the decalin in the sheet was extracted while continuously immersing the heat-set sheet in a methylene chloride bath divided into two tanks for 30 seconds each. After carrying out the sheet from the methylene chloride bath, methylene chloride was dried and removed under a temperature atmosphere of 40 ° C., and annealed while being conveyed on a roller heated to 120 ° C. Thus, the polyethylene microporous membrane according to this embodiment was obtained.
  • Plasma treatment (Nordson MARCH AP-300: output 150 W, treatment pressure 400 mTorr, gas flow 160 sccm, treatment time 135 seconds) was performed on both sides of the polyethylene microporous membrane.
  • the hydrophilic polyethylene microporous membrane according to this embodiment was obtained.
  • a PET film with an adhesive was attached to one surface of the hydrophilic polyethylene microporous membrane to obtain a laminate.
  • Examples 2-4, Comparative Examples 1-2 A polyethylene microporous membrane, a hydrophilic polyethylene microporous membrane, and a laminate were produced in the same manner as in Example 1 except that the composition of the polyethylene solution or the production process of the microporous membrane was changed as shown in Table 1.
  • a PET film was attached to the surface of the polyethylene microporous membrane on the side not subjected to the plasma treatment.
  • the film thickness of the polyolefin microporous film was determined by measuring 20 points with a contact-type film thickness meter (manufactured by Mitutoyo Co., Ltd.) and averaging them.
  • a contact-type film thickness meter manufactured by Mitutoyo Co., Ltd.
  • the measurement pressure was 0.1N.
  • X-ray CT device Rigaku's high-resolution 3DX X-ray microscope, trade name "nano3DX"
  • X-ray source Cu
  • X-ray camera L0270
  • X-ray tube voltage / tube current 40 kV-30 mA CT imaging range: 0 ° to 180 °
  • the curvature ratio ( ⁇ X , ⁇ Y , ⁇ Z ) and the permeability index (T X , T) of the microporous polyolefin membrane are determined by the above-described image analysis and simulation.
  • Y , TZ was calculated, and ⁇ X / ⁇ Z , ⁇ Y / ⁇ Z , T X / T Z, and T Y / T Z were calculated.
  • ⁇ Z is the curvature ratio in the thickness direction
  • ⁇ X is the curvature ratio in the TD direction
  • ⁇ Y is the curvature ratio in the MD direction.
  • T Z was a transparency index in the thickness direction
  • T X was a transparency index in the TD direction
  • T Y was a transparency index in the MD direction.
  • 2A to 2E show cross-sectional images obtained from X-ray CT of the polyolefin microporous membranes of Examples 1 to 3 and Comparative Examples 1 and 2.
  • X is the TD direction
  • Y is the MD direction
  • Z is the thickness direction.
  • the white straight line in each image of FIGS. 2A to 2E is a scale bar
  • the scale bar in the image in the XY direction shows 50 ⁇ m
  • the scale bar in the image in the XZ direction shows 20 ⁇ m
  • the scale in the image in the YZ direction shows 20 ⁇ m
  • the bar indicates 20 ⁇ m.
  • the constituent materials are a, b, c, ..., N
  • the masses of the constituent materials are Wa, Wb, Wc, ..., Wn (g / cm 2 )
  • the true densities of the constituent materials are xa.
  • the air permeation time (second / 100 mL) of the polyolefin microporous membrane having an area of 642 mm 2 is measured, and the air permeation time is divided by the film thickness ( ⁇ m) of the polyolefin microporous membrane per 1 ⁇ m in thickness.
  • the air permeation time (second / 100 mL ⁇ ⁇ m) was determined.
  • the polyolefin microporous membrane was cut out in a MD direction of 10 cm ⁇ TD direction of 10 cm, immersed in ethanol, lifted from ethanol, and dried at room temperature.
  • the dried polyolefin microporous membrane was set in a stainless circular liquid-permeable cell having a liquid-permeable area of 17.34 cm 2 .
  • 100 mL of ethanol is permeated at a differential pressure of 92 kPa to 95 kPa, and the time required for permeation of 100 mL of ethanol (sec ) was measured.
  • the measurement was performed in a temperature atmosphere of room temperature of 24 ° C.
  • the ethanol flow rate (mL / (min ⁇ cm 2 ⁇ MPa)) is calculated by converting the measurement conditions and the measured value into a unit, and the ethanol flow rate and the film thickness ( ⁇ m) of the polyolefin microporous film measured in advance are calculated. Multiplied.
  • the maximum puncture load (g) was measured by performing a needle penetration test (needle: radius of curvature of tip 0.5 mm, puncture speed: 320 mm / min) using the Tensilon universal material testing machine (RTE-1210), and maximum puncture load was divided by the film thickness ( ⁇ m) of the polyolefin microporous film to obtain the puncture load (g / ⁇ m) per 1 ⁇ m in thickness.
  • Tris-hydrochloric acid buffer solution (Tris-HCl, pH 8.2) (0.6 mL) was evenly applied to a 150 mm ⁇ 18 mm ⁇ 340 ⁇ m cellulose pad (Ahlstrom), and the temperature was 50 ° C. And dried for 1 hour to obtain a sample pad 2.
  • a chromatography carrier 1, a conjugate pad 3, a sample pad 2 and an absorption pad 4 are provided on a support 5 (a backing sheet made by Lohmann, 150 mm ⁇ 60 mm) having an adhesive applied on one surface.
  • a support 5 a backing sheet made by Lohmann, 150 mm ⁇ 60 mm
  • the overlapping width of the sample pad 2 and the conjugate pad 3 is 4 mm
  • the overlapping width of the conjugate pad 3 and the chromatography carrier 1 is 2 mm
  • the overlapping width of the chromatography carrier 1 and the absorption pad 4 is 5 mm.
  • the detection unit 11 of No. 1 was arranged closer to the absorption pad 4 than the conjugate pad 3.
  • the entire composite sheet is cut into 5 mm widths in the length direction, and an immunochromatographic strip A (total length 60 mm in the developing direction, width 5 mm.
  • the TD direction of the hydrophilic polyethylene microporous membrane is the sample developing direction). Obtained.
  • a sample was prepared by diluting the hCG antigen (substance to be detected) to 16.7 nkat in a phosphate buffer containing 1% by mass of BSA and 0.095% by mass of NaN 3 .
  • a sample (100 ⁇ L) is dropped onto the sample pad 2 of the strip A for immunochromatography to be developed, and an LED (light emitting diode) whose emission peak wavelength is around 520 nm is used by using an immunochromatographic reader (manufactured by Hamamatsu Photonics, model number C10066-10). Was used as a light source, and the absorbance in the detection unit 11 was measured with time.
  • FIG. 3 shows changes in absorbance with time in Example 2 and Comparative Example 1.
  • a red line can be clearly confirmed on the detection part.

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Abstract

Un film microporeux de polyoléfine dans lequel l'épaisseur de film est de 1 à 400 µm et qui satisfait les formules (1) et (2) ou satisfait les formules (3) et (4). Formule (1): 0.7 ≤ τXZ ≤ 1.5 Formule (2): 0.7 ≤ τYZ ≤ 1.5 τX: Tortuosité dans une première direction le long d'une surface du film microporeux de polyoléfine τY: Tortuosité dans une seconde direction le long de la surface du film microporeux de polyoléfine τZ: La tortuosité dans le sens de l'épaisseur de la formule de film microporeux de polyoléfine (3) : 0.5 ≤ TX/TZ ≤ 2.0 Formule (4): 0.5 ≤ TY/TZ≤ 2.0 TX: Indice de perméabilité dans la première direction le long de la surface du film microporeux de polyoléfine TY: Indice de perméabilité dans la seconde direction le long de la surface du film microporeux de polyoléfine TZ: L'indice de perméabilité dans la direction de l'épaisseur du film microporeux de polyoléfine
PCT/JP2019/041768 2018-10-26 2019-10-24 Film microporeux de polyoléfine, filtre, support de chromatographie et bande pour immunochromatographie WO2020085449A1 (fr)

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