JP4182087B2 - Liquid absorption performance measuring method and liquid absorption performance measuring apparatus - Google Patents

Description

  The present invention relates to a method for measuring liquid absorption performance and an apparatus for measuring liquid absorption performance.

Cylinder (2) arranged such that the bottom is closed with a filter medium (1) that allows liquid to pass without passing liquid-absorbing particles, and the cylinder axial direction is vertical;
A piston (4) which can be freely inserted into the cylinder (2) and has a liquid inlet (3) at the bottom;
A weight (5) that can be uniformly pressurized to (4); and a space (6) in which liquid-absorbing particles can be arranged between the top surface of (1) and the bottom surface of (4), A liquid absorption amount measuring device is known in which the ratio (S1 / S2) of the filtration area (S1) of (1) to the opening area (S2) of (3) is 2 to 10,000 (patent) Reference 1).
JP 2005-098956 A

In the conventional measuring device, the correlation with the liquid absorbency in actual use is insufficient, and the liquid absorbent article (paper napkin) manufactured using the liquid-absorbing particles that showed good liquid absorbency in the conventional measuring device. And paper diapers, etc.) have a problem that liquid absorption may be extremely poor.
That is, an object of the present invention is to provide a liquid absorption amount measuring apparatus and a liquid absorption amount measuring method that are highly correlated with the liquid absorption property in actual use.

The inventors of the present invention have reached the present invention as a result of intensive studies to achieve the above object.
That is, the characteristics of the method for measuring the liquid absorption performance of the present invention are:
A cylindrical container (50) comprising a cylindrical part (20) having a liquid discharge port (10) and a circular bottom part (40) having a liquid discharge part (30) at least on the outer peripheral part is erected so that the cylindrical axis is vertical. After putting the measurement sample into this cylindrical container (50),
A piston (90) composed of a cylindrical part (70) having a liquid discharge part (60) and a filter medium part (80) is inserted into the cylindrical container (50), and a liquid inlet at the top of the cylindrical part (70) is inserted. Inject liquid from (100)
The amount of liquid injected before the liquid flows out from the liquid outlet (10) and / or the liquid outlet (30); and / or the liquid flowing out from the liquid outlet (10) and / or the liquid outlet (30) The point is to measure the amount of.

The feature of the liquid absorption performance measuring device of the present invention is
An apparatus for measuring the liquid absorption performance of liquid absorbent particles,
A cylindrical container (50) comprising a cylindrical part (20) having a liquid discharge port (10) and a circular bottom part (40) having a liquid discharge part (30) at least on the outer periphery;
A piston (90) comprising a cylindrical part (70) having a liquid discharge part (60) and a liquid inlet (100), and a filter medium part (80);
The point is that

The measurement method of the liquid absorption performance of the present invention can obtain a measurement result having a very high correlation with the liquid absorption in actual use. Moreover, when the liquid absorption performance measuring device of the present invention is used, a measurement result having a very high correlation with the liquid absorption in actual use can be obtained.
Therefore, if the liquid-absorbing particles exhibiting good liquid-absorbing performance by the liquid-absorbing performance measuring apparatus or the liquid-absorbing performance measuring method of the present invention are used, good liquid absorbency is exhibited even in actual use.

The cylindrical container (50) includes a cylindrical portion (20) and a circular bottom portion (40), and one of the two open portions (upper end open portion and lower end open portion) of the cylindrical portion (20) (lower end open portion). ) Is closed at the circular bottom (40).
The cylindrical portion (20) has a liquid discharge port (10), and is configured so that a part of the liquid used for measurement can be discharged to the outside of the cylindrical container (50).
There is no restriction | limiting in the shape of a liquid discharge port (10), Any may be circular, an ellipse, a rectangle, a hexagon, etc.
The size (mm ² ) of the liquid discharge port (10) is preferably 0.01 to 100, more preferably 0.2 to 70, particularly preferably 1 to 50, more particularly preferably 5 to 30, and most preferably. 10-20.
The number of the liquid outlets (10) is preferably 4 to 10,000, more preferably 10 to 5,000, particularly preferably 100 to 1,000, and most preferably 200 to 500 or more.
The position of the liquid discharge port (10) is not limited, but it is preferably arranged uniformly in the cylindrical portion (21), more preferably arranged with regularity.

The inner diameter (mm) of the cylindrical portion (20) is preferably 30 to 500, more preferably 40 to 400, particularly preferably 50 to 300, and most preferably 60 to 200, from the viewpoint of the installation space of the measuring device. .
The length (mm) of the cylindrical portion (20) is preferably 20 to 500, more preferably 30 to 400, particularly preferably 40 to 300, and most preferably 50 to 200, from the viewpoint of the installation space of the measuring device. is there.
Although there is no restriction | limiting as a material of a cylindrical part (20), From a viewpoint of internal observation of a cylindrical container (50), a transparent thing is preferable, for example, glass and plastics (vinyl chloride, polycarbonate, polypropylene, polyethylene, etc.) Etc. are preferred.

Instead of providing the liquid discharge port (10), the cylindrical part (20) may be configured by entirely of the cylindrical part (20), or a part of the cylindrical part (20) may be configured by the filter medium. .
The filter medium is not limited as long as it can easily pass through a liquid, and includes fibers (paper, cotton, hemp, etc.), inorganic porous bodies (ceramics, glass filters, etc.), nets (wire mesh, nylon mesh, etc.) and the like.

  When a part of the cylindrical portion (20) is formed of a filter medium, the cylindrical portion (20) is not limited as long as the liquid is discharged from the cylindrical container (50) to the outside. For example, a structure that can be constructed by filling the liquid discharge port (10) with a filter medium; a cylinder that is composed of a material similar to the above (glass, plastic, etc.) and a cylinder that is composed of the filter medium are vertically coupled. Structure to be obtained; Structure that can be constructed by repeatedly joining up and down a cylinder made of the same material (glass, plastic, etc.) and a cylinder made of a filter medium (preferably about 2 to 1000 bonds); And a structure that can be formed into a cylinder by repeatedly joining a plate-like body (barrel plate) made of the same material (glass, plastic, etc.) and a plate-like body (barrel plate) made of filter media to the left and right. (The number of bonds is preferably about 4 to 1000).

Among these, from the viewpoint of the strength of the cylindrical portion (20), etc., the structure in which the liquid discharge port (10) is provided; the liquid discharge port (10) provided in the cylindrical portion (20) may be filled with a filter medium. A structure in which all of the cylindrical part (20) is made of a filter medium, and more preferably a structure in which the liquid discharge port (10) provided in the cylindrical part (20) is filled with the filter medium; and the cylindrical part A structure in which all of (20) is made of a filter medium, particularly preferably a structure in which all of the cylindrical portion (20) is made of a filter medium.
When a part or all of the cylindrical portion (20) is constituted by a filter medium, the thickness (mm) of the filter medium is preferably 0.1 to 100, more preferably 0.5 to 50, particularly preferably 1 to 30, most preferably. Preferably it is 2-10. Within this range, the correlation with actual use is further improved.

The circular bottom part (40) has a liquid discharge part (30) at least on the outer peripheral part, and is configured so that a part of the liquid used for measurement can be discharged outside the cylindrical container (50).
The outer peripheral portion means a portion (donut-shaped portion) of the circular bottom portion (40) excluding a circle that is concentric with the center of the circular bottom portion (40) and smaller than the radius of the circular bottom portion (40).
The ratio (%) of the area of the liquid discharge part (30) to the circular bottom part (40) is preferably 0.5 to 50, more preferably 1 to 40, particularly preferably 5 to 30, and most preferably 10 to 20. is there.
If the liquid discharge part (30) is comprised so that a part of liquid used for a measurement can be discharged | emitted outside a cylindrical container (50), the whole or a part of liquid discharge part (30) will be a filter medium. It may be configured by providing a liquid discharge port (same in shape and size) as the liquid discharge port (10).

When a part of the liquid discharge part (30) is constituted by a filter medium, the liquid discharge part (30) is not limited as long as the liquid is discharged from the cylindrical container (50) to the outside. For example, the structure etc. which can be comprised by filling a liquid discharge port with a filter medium are mentioned.
Among these, a structure in which the entire liquid discharge part (30) can be configured with a filter medium; and a structure in which a liquid discharge port can be provided like the liquid discharge port (10) are preferable, and a liquid discharge part ( The whole of 30) is a structure that can be composed of a filter medium.

When the liquid discharge port (30) is provided with a liquid discharge port, the number of the liquid discharge ports is preferably 4 to 10,000, more preferably 10 to 5000, particularly preferably 100 to 1000, and most preferably 200 to 500. That's it.
When a part or all of the liquid discharge part (30) is configured with a filter medium, the thickness (mm) of the filter medium is preferably 0.1 to 100, more preferably 0.5 to 50, and particularly preferably 1 to 30, Most preferably, it is 2-10. Within this range, the correlation with actual use is further improved.

The diameter (mm) of the circular bottom (40) is preferably 30 to 500, more preferably 40 to 400, particularly preferably 50 to 300, and most preferably 60 to 200, from the viewpoint of the installation space of the measuring device. .
Of the circular bottom portion (40), the same material as that of the cylindrical portion (21) can be used as a material other than the liquid discharge portion (30).

  The cylindrical container (50) is erected so that the cylindrical axis is in the vertical direction (gravity axis direction), but does not require a high degree of verticality, and the piston (90) can fall inside the cylindrical container (50). It's okay.

The piston (90) includes a cylindrical part (70), a filter medium part (80), and a liquid inlet (100), and one of the two open parts (upper end open part and lower end open part) of the cylindrical part (70). One (lower end open part) is configured to be blocked by the filter medium part (80). The piston (90) is inserted into the cylindrical container (50) to form a sealed space for the measurement sample.
The filter medium part (80) may be larger than the lower end opening part of the cylindrical part (70), but the diameter of the filter medium part (80) is preferably slightly smaller than the inner diameter of the cylindrical container (50).

  The difference (mm) between the diameter of the filter medium portion (80) {diameter including this when a slip member (120) described later is provided)} and the inner diameter of the cylindrical container (50) is preferably 0.1 to 4, Preferably it is 0.2-3, Most preferably, it is 0.3-2, Most preferably, it is 0.4-1. Within this range, the piston (90) can be more easily dropped into the cylindrical container (50), and the correlation with actual use is further improved.

  The thickness (mm) of the filter medium part (80) is preferably 0.1 to 100, more preferably 0.5 to 50, particularly preferably 1 to 30, and most preferably 2 to 10. Within this range, the correlation with actual use is further improved.

The shape of the filter medium part (80) is not limited as long as it can be inserted into the cylindrical part (20), but most of the liquid discharged from the liquid discharge part (60) described later is discharged from the liquid discharge port (10). It is preferable that {the upper surface portion of the filter medium portion is inclined from the center portion to the outer peripheral portion (the upper surface portion is mountain-like, bowl-shaped or twisted}).
A sliding member (120) may be provided on the outer periphery of the filter medium part (80) so that the piston (90) can move smoothly in the cylindrical container (50).
Examples of the sliding member (120) include Teflon, polyethylene, propylene, vinyl chloride, and silicone resin.
When the sliding member (120) is provided, the vertical thickness {thickness of the outer peripheral portion of the filter medium part (80)} may be within the range of the thickness of the filter medium part (80).
When the sliding member (120) is provided, the horizontal thickness {width of the donut ring} is preferably thin, and is about 0.01 to 5 mm.

  The cylindrical part (70) has a liquid discharge part (60) and a liquid injection port (100), and is configured so that a part of the liquid used for measurement can be discharged to the outside of the piston (90). That is, the liquid discharge part (60) is configured to discharge, out of the liquid injected from the liquid inlet (100), the liquid that does not pass through the filter medium part (80) and overflows to the outside of the piston (90). . Then, this liquid is absorbed, diffused or dropped into the measurement sample through the filter medium part (80) (when the filter medium part (80) is larger than the lower end open part of the cylindrical part (70)), and further passes through the filter medium part (80). The liquid that has not been discharged is discharged from the liquid discharge port (10) to the outside of the cylindrical container (50).

The liquid discharge part (60) has the same structure as the liquid discharge port (10).
The ratio (%) of the area of the liquid discharge part (60) to the cylindrical part (70) is preferably 0.1 to 50, more preferably 1 to 40, particularly preferably 5 to 30, and most preferably 10 to 20. is there.
Although there is no restriction | limiting in the position of a liquid discharge part (60), It is preferable that it exists within 100 mm from the lower end part of a cylindrical part (70), More preferably, it is within 50 mm, Most preferably, it is within 40 mm, Most preferably, it arrange | positions within 30 mm. It is to be done.

In order to prevent the liquid injected from the liquid injection port (100) from being discharged directly from the liquid discharge part (60), a back pressure valve is provided in the liquid discharge part (60), or an umbrella shape is formed on the upper part of the liquid discharge part (60). It is preferable to provide a member (110).
Although there is no restriction | limiting as an umbrella-shaped member (110), For example, the member which is illustrated by FIG. 1 and 7 grade | etc., Is applicable.

The inner diameter (mm) of the cylindrical portion (70) is preferably 30 to 500, more preferably 40 to 400, particularly preferably 50 to 300, and most preferably 60 to 200, from the viewpoint of the installation space of the measuring device. .
The length (mm) of the cylindrical portion (70) is preferably 20 to 500, more preferably 30 to 400, particularly preferably 40 to 300, and most preferably 50 to 200 from the viewpoint of the installation space of the measuring device. is there.
The material of the cylindrical portion (70) is not limited, but from the viewpoint of internal observation of the cylindrical portion (70), a transparent one is preferable, and the same one as the cylindrical container (50) is preferable.

The liquid injection port (100) is arranged in the upper part of the cylindrical part (70), and is configured to inject liquid into the cylindrical part (70) and supply the liquid to a part of the measurement sample.
The liquid inlet (100) may use the upper end opening of the cylindrical portion (70) as it is as the liquid inlet (100).
The liquid inlet (100) may be connected to a pipe connected to the metering pump, and such a pipe may be inserted.
The inner diameter (mm) of the liquid injection port (100) is preferably 1 to 300, more preferably 2 to 100, particularly preferably 3 to 70, and most preferably 4 to 50, from the viewpoint of the installation space of the measuring device. is there.

The ratio (S1 / S2) between the cross-sectional area (S1) of the liquid outlet (30) and the cross-sectional area (S2) of the liquid inlet (100) is not particularly limited, but is preferably 1 to 10,000, more preferably 10 To 1000, particularly preferably 30 to 100, most preferably 50 to 60. Within this range, the correlation with actual use is further improved.
The liquid absorption performance measuring device of the present invention is provided with a guide in the cylindrical portion (70) in addition to the devices shown in Examples 1 to 11 (FIGS. 1 to 11), and the cylindrical portion (70) does not shake from side to side. You may use the piston (FIG. 14) comprised so that the whole cylindrical part (70) might adjoin the cylindrical container (50) like the made piston (FIGS. 12-13) and a syringe.

Next, the measuring method of the liquid absorption performance of this invention is demonstrated to each operation order (1-5).
When a liquid is supplied to a part of the measurement sample, it is diffused, dropped and absorbed by the measurement sample other than the part supplied while diffusing, dropping and absorbing the liquid, but when the supply amount of the liquid exceeds a certain amount ( The liquid overflows when the measurement sample's diffusion capacity, drop capacity, and absorption capacity of the liquid are exceeded.
On the other hand, when the absorption capacity of the measurement sample with respect to the liquid is low, most of the liquid passes through (diffuses or drops) the measurement sample layer without being absorbed by the measurement sample.
The liquid absorption performance measuring method of the present invention is intended to quantitatively grasp the absorption capacity, diffusion capacity and drop capacity of the measurement sample by measuring the amount of the overflowing liquid and the amount of the liquid passing through. It is.

1. After confirming that no liquid or the like is attached to the measurement device, the measurement sample is put into the cylindrical container (50).
Although there is no restriction | limiting as a measurement sample, It is preferable that a liquid-absorbing particle (A) is included.
The weight average particle diameter (μm) of the liquid-absorbent particles (A) is not particularly limited, but is preferably 50 to 1000, more preferably 70 to 900, particularly preferably 100 to 800, still more preferably 150 to 750, Most preferably, it is 200-700.
In addition, the weight average particle diameter is determined by using a conventional method, for example, a low tap test sieve shaker and a standard sieve (JIS Z8801-1: 2000), Perry's Chemical Engineers Handbook, 6th edition (MacGlow Hill). * Book cum bunny, 1984, p. 21). That is, the JIS standard sieves are 1000 μm, 850 μm, 710 μm, 500 μm, 425 μm, 355 μm, 250 μm and 150 μm from the top, and the order of the saucer, or 500 μm, 355 μm, 250 μm, 150 μm, 125 μm, 75 μm and 45 μm, and the saucer from the top. Combine in order. About 50 g of the measured particles are put in the uppermost screen and shaken for 5 minutes with a low-tap test sieve shaker. Weigh the measured particles on each sieve and the pan, and calculate the weight fraction of the particles on each sieve by taking the total as 100% by weight. Use this value as a logarithmic probability paper [horizontal axis is sieve aperture (particle size ), After the vertical axis is plotted on the weight fraction], a line connecting the points is drawn to obtain a particle diameter corresponding to the weight fraction of 50% by weight, and this is defined as a weight average particle diameter.

The apparent density (g / cm ³ ) of the liquid-absorbent particles (A) is not particularly limited, but is preferably 0.2 to 1.0, more preferably 0.3 to 0.8, and particularly preferably 0.4. -0.7, most preferably 0.5-0.6. Within this range, the correlation with actual use is further improved. The apparent density (g / cm ³ ) is measured according to ISO 9136.

The liquid absorbing particles (A) include liquid absorbing organic particles and liquid absorbing inorganic particles.
Examples of the liquid-absorbing organic particles include known high water-absorbing resins.
Examples of the liquid-absorbing inorganic particles include silica gel, zeolite, layered clay, talc and activated carbon.
Of these liquid-absorbing particles (A), the liquid-absorbing particles (A) are preferably applicable to liquid-absorbing organic particles, and more preferably suitable for particles composed of a highly water-absorbing resin and a water-absorbing resin.

The measurement sample is preferably prepared by uniformly mixing the liquid-absorbing particles (A) and the fine particles (B) having a weight average particle diameter of 100 to 700 μm.
The weight average particle diameter (μm) of the fine particles (B) is preferably 100 to 700, more preferably 150 to 600, particularly preferably 200 to 550, still more preferably 250 to 500, and most preferably 300 to 400. . Within this range, the correlation with actual use is further improved.

The apparent density (g / cm ³ ) of the fine particles (B) is not particularly limited, but is preferably 0.001-1, more preferably 0.01-0.5, particularly preferably 0.05-0.1, Most preferably, it is 0.06-0.08. Within this range, the correlation with actual use is further improved.

The fine particles (B) include inorganic fine particles and organic fine particles.
Examples of the inorganic fine particles include fine powder silica, glass balloon, shirasu balloon, silicone beads, zinc fine particles, copper fine particles, stainless fine particles, and steel fine particles.
Examples of the organic powder include styrene beads, ethylene beads, silicone fine particles, and pulp.
Among these fine particles (B), inorganic fine particles are preferable from the viewpoint of easy uniform mixing with the liquid-absorbing particles (A), more preferably fine powder silica and shirasu balloons, particularly preferably shirasu balloons. is there.

When the measurement sample is prepared by uniformly mixing the liquid-absorbing particles (A) and the fine particles (B), the content (% by weight) of the liquid-absorbing particles (A) is the liquid-absorbing particles (A). Based on the weight of the fine particles (B), 10 to 90 is preferable, more preferably 20 to 80, particularly preferably 30 to 70, and most preferably 40 to 60. In this case, the content (% by weight) of the fine particles (B) is preferably 10 to 90, more preferably 20 to 80, particularly based on the weight of the liquid-absorbing particles (A) and the fine particles (B). Preferably it is 30-70, Most preferably, it is 40-60.
When the measurement sample is prepared by uniformly mixing the liquid-absorbing particles (A) and the fine particles (B), the liquid-absorbing particles (A) and the fine particles (B) are not limited as long as they are uniformly mixed. For example, uniform mixing can be performed using a mixer (Nobilta manufactured by Hosokawa Micron Corporation).

The input amount of the measurement sample is preferably such an amount that the thickness (mm) of the measurement sample becomes 0.5 to 10 when the thickness is adjusted to a uniform thickness on the circular bottom (40) in the next step, and more preferably 1 to 1. 8, particularly preferably 2-5, most preferably 3-4. Within this range, the correlation with actual use is further improved. For example, when the measurement sample has the above-described weight average particle diameter and apparent density {including the case where the measurement sample is prepared by uniformly mixing the liquid-absorbing particles (A) and the fine particles (B)}, The input amount (mg / cm ² ) is preferably 20 to 200, more preferably 30 to 100, particularly preferably 35 to 80, and most preferably 40 to 60. Within this range, the correlation with actual use is further improved.

2. The measurement sample put into the cylindrical container (50) is adjusted to a uniform thickness on the circular bottom (40). There is no limitation on the method for adjusting the thickness as long as the thickness is almost uniform. For example, a slight vibration is applied to a cylindrical container (50) or a circular bottom (40), such as a vibrator (for example, a vortex rack or a deep well rack in Tokyo. The method given by Science Instruments Co., Ltd.) can be applied.

3. Next, the piston (90) is inserted into the cylindrical container (50) so that the filter medium part (80) of the piston (90) is in contact with the measurement sample.
The measurement sample can be in a pressurized state, and when measured in a pressurized state, it can be weighted through this piston (90).
The method of weighting is not limited, but a method or weight using a hydraulic application device (for example, a hydraulic pressurization device manufactured by NPA System) or a pneumatic application device (for example, a reciprocating compressor manufactured by Anest Iwata) is applied. Methods etc. can be applied. Of these, from the viewpoint of simplicity, a method of applying a weight is preferable. A weight role may be added to the piston (90) itself.
The pressure (g / cm ² ) applied to the measurement sample is preferably 1 to 300, more preferably 3 to 100, particularly preferably 5 to 50, and most preferably 10 to 30. Within this range, the correlation with actual use is further improved.

4). The liquid is poured from the liquid inlet (100) at the top of the cylindrical portion (70).
The liquid is not limited as long as it can be absorbed by the measurement sample, and includes an oily liquid and an aqueous liquid.
As the oily liquid, a silicone oil having a kinematic viscosity (m ² / s) at 40 ° C. of 5 × 10 ⁻⁷ to 2 × 10 ⁻³ , and a kinematic viscosity at 40 ° C. of 5 × 10 ⁻⁶ to 4 × 10 ^−4. Mineral oil, paraffin oil having kinematic viscosity at 40 ° C. of 1 × 10 ⁻⁶ to 1 × 10 ⁻³ , animal and vegetable oils (rapeseed oil, sunflower oil, beef tallow and lard) and esters having 6 to 15 carbon atoms (dibutyl) At least one selected from the group consisting of phthalates and the like.

Examples of the aqueous liquid include physiological saline (0.9% by weight sodium chloride aqueous solution), artificial urine (calcium chloride 0.03% by weight, magnesium sulfate 0.08% by weight, sodium chloride 0.8% by weight, and deionized water 99). 0.09% by weight aqueous solution), distilled water, deionized water, tap water, blood, urine, seawater, river water, and lake water.
Of these liquids, aqueous liquids are preferred, more preferably at least one selected from the group consisting of physiological saline, artificial urine, deionized water, tap water, blood, urine, seawater, river water and lake water, in particular. Preferably, at least one selected from the group consisting of physiological saline, artificial urine, deionized water, tap water, blood and seawater, most preferably selected from the group consisting of physiological saline, artificial urine, deionized water and blood. At least one.

The liquid to be poured may be poured all at once or continuously or intermittently. Further, in the case of continuous injection, there may or may not be a pulsating flow, but it is important to always have the same pouring method. From such a viewpoint, the liquid is preferably poured continuously or intermittently, more preferably continuously poured, and particularly preferably continuously poured without a pulsating flow.
When pouring continuously or intermittently, it may be supplied using a syringe or beaker and a watch, and may be supplied using a metering pump (gear pump, tube pump, impeller pump, syringe pump, etc.), etc. From the viewpoint of quantitative accuracy, it is preferable to use a quantitative pump.
When pouring continuously or intermittently, the inflow amount of liquid (ml / min) is preferably 1 to 1000, more preferably 3 to 500, particularly preferably 5 to 200, and most preferably 10 to 100. . Within this range, the correlation with actual use is further improved.

5. The amount of liquid injected (W10) from the beginning of pouring the liquid until the liquid flows out from the liquid outlet (10) or the filter medium cylinder (22) and / or the liquid outlet (30);
In addition, the amount (W20) of the liquid flowing out from the liquid discharge port (10) or the filter medium cylindrical portion (22) and / or the liquid discharge port (30) is measured.
The amount of liquid injected (W10) may be calculated from the time (T) from the start of pouring the liquid until the liquid flows out and the inflow amount of the liquid.
The amount of liquid flowing out (W20) is the amount of liquid flowing out from the liquid discharge port (10) or the filter medium cylindrical portion (22) (W21) and the amount of liquid flowing out from the liquid discharge port (30) (W22). ) And may be weighed separately.
The amount of the overflowing liquid described at the beginning of the description of the method for measuring the liquid absorption performance of the present invention corresponds to the amount of liquid (W21). Similarly, the amount of liquid passing through the measurement sample layer corresponds to the amount of liquid (W22).

    The measurement method of the present invention is preferably carried out at a constant temperature, more preferably a temperature close to the temperature in actual use (the difference from the temperature in actual use is preferably within 15 ° C., more preferably within 10 ° C. Particularly preferably within 5 ° C.). For example, when the measurement sample contains liquid absorbent particles for disposable diapers, the measurement temperature (° C.) is preferably 22 to 52, more preferably 27 to 47, and particularly preferably 30 to 40.

Hereinafter, although an example and a comparative example explain the present invention further, the present invention is not limited to these. Hereinafter, unless otherwise specified, “part” means “part by weight” and “%” means “% by weight”. The unit indicating the size of the device means millimeter (mm).
<Example 1>
<Measurement device>
A cylindrical portion (20) composed of a glass filter plate having a thickness of 5 mm and an inner diameter of 60 mm (corresponding to the pore size of 100 to 120 μm in FIG. 63 with JIS R3503-1994; the same shall apply hereinafter);
From a rigid vinyl chloride disc (diameter 30 mm, thickness 5 mm) and a cylindrical bottom part (40) composed of a donut-shaped glass filter plate {diameter 60 mm, inner diameter 30 mm, thickness 5 mm; liquid discharge part (30)}, A circular container (50) was created (FIGS. 1-3).
On the other hand, four circular holes {liquid discharge part (60)} having a diameter of 5 mm are provided at equal intervals so as to contact the lower end of a rigid vinyl chloride cylinder (inner diameter 20 mm, length 50 mm, thickness 5 mm). An umbrella-shaped member (110) made of a hard vinyl chloride donut-shaped ring (ring width: 3 mm, outer peripheral side thickness: 5 mm, inner week side thickness: 3 mm) is placed 10 mm above the liquid discharge part (60) inside the vinyl chloride cylinder. A provided cylindrical portion (70);
A sliding member composed of a Teflon donut ring (diameter 59 mm, inner diameter 55 mm, thickness 3 mm) on a glass filter plate (diameter 55 mm, thickness of the portion in contact with the cylindrical portion 70 is 8 mm, outer periphery 3 mm) The piston (90) was created from the filter medium part (80) provided with (120) (FIGS. 1 and 4 to 6).
And the cylindrical container (50) stands up so that the cylinder axis is in the vertical direction (gravity axis direction), and the piston (90) is inserted into the cylindrical container (50), whereby the liquid absorption performance measuring device of the present invention. (AME1) was created.

<Measurement sample>
50 parts of liquid-absorbing particles (A1) to (A15) obtained in the same manner as in <Synthesis Example 1> to <Comparative Synthesis Example 3> described in Patent Document 1, and fine particles (B1) {Aerosil 200PE, Nippon Aerosil 50 parts of Silica Co., Ltd. were mixed for 2 minutes at 25 ° C. using Nobilta (Hosokawa Micron mixer) to prepare measurement samples (1) to (15).

<Measurement>
In a cylindrical container (50), 2.00 g of a measurement sample was charged and adjusted to a uniform thickness on a wire mesh.
Next, the piston (90) is inserted into the cylindrical container (50) so as to come into contact with the measurement sample, and a measurement sample is uniformly pressurized by placing a doughnut-shaped weight of 0.25 kg, and then the upper portion of the cylindrical portion (70). 100 ml of physiological saline was poured from the {liquid inlet (100)} at a constant flow rate of 10 ml / min.
And time (T, second) until physiological saline leaked from a cylindrical container (50) was measured. Moreover, the weight (W20) of the physiological saline leaked from the cylindrical container (50) was measured, and the amount of liquid (ml / g) absorbed by 1 g of the liquid-absorbing particles (A1) to (A15) from the following formula ( W10) was calculated. And these operations were repeated 5 times and the average value of 5 times was shown in Table 1. In addition, the measurement was performed at 25 ± 2 ° C. (in a constant temperature room).

（ＲＡＰ）は、測定試料の重量に基づく、吸液性粒子（Ａ）〜（Ａ１５）の含有量（％）である。

(RAP) is the content (%) of the liquid-absorbing particles (A) to (A15) based on the weight of the measurement sample.

<Example 2>
The liquid absorbing particles (A1) to (A15) 50 parts and the fine particles (B1) 50 parts were changed to (A1) to (A15) 30 parts and (B1) 70 parts in the same manner as in Example 1, except that the liquid The average value of the amount (W10) is shown in Table 1.

<Example 3>
The liquid absorbing particles (A1) to (A15) 50 parts and the fine particles (B1) 50 parts were changed to (A1) to (A15) 70 parts and (B1) 30 parts in the same manner as in Example 1, except that the liquid The average value of the amount (W10) is shown in Table 1.

<Example 4>
Table 1 shows the average value of the amount of liquid (W10) in the same manner as in Example 1 except that the fine particles (B1) were changed to the fine particles (B2) {KC floc W-400G, pulp manufactured by Nippon Paper Chemicals Co., Ltd.}. .

<Example 5>
The average value of the amount of liquid (W10) is shown in Table 1 in the same manner as in Example 1 except that the fine particles (B1) were changed to the fine particles (B3) {No. 2 for processing, Shirasu balloon made by Mitsui Mining & Smelting Co., Ltd.}. .

<Example 6>
The average value of the amount of liquid (W10) is shown in Table 1 in the same manner as in Example 1 except that the fine particles (B1) were changed to the fine particles (B4) {Nitto Zeolite No. 1, zeolite manufactured by Nitto Flour Industries Co., Ltd.}. .

<Example 7>
Table 1 shows the average value of the amount of liquid (W10) in the same manner as in Example 1 except that the physiological saline was changed to artificial urine.

<Example 8>
Table 1 shows the average value of the amount of liquid (W10) in the same manner as in Example 1, except that the donut weight (0.25 Kg) was changed to the donut weight (0.50 Kg).

<Example 9>
Table 1 shows the average value of the amount of liquid (W10) in the same manner as in Example 1 except that the flow rate of physiological saline was changed to 20 ml / min.

<Example 10>
Minerals whose liquid-absorbing particles (A1) to (A15) were changed to Uremer (urea resin manufactured by Meito Chemical Co., Ltd.) and whose kinematic viscosity (m ² / s) at 40 ° C. was 5 × 10 ⁻⁶ Table 1 shows the average value of the amount of liquid (W10) in the same manner as in Example 1 except that the oil was changed.

<Example 11>
<Measurement device>
As shown in FIG. 8, a cylindrical portion (20 having a rigid vinyl chloride cylinder (inner diameter 60 mm, thickness 5 mm, length 125 mm) provided with 324 liquid discharge ports (10) each having a circular hole (diameter 3 mm). ) From a hard vinyl chloride disc (diameter 30 mm, thickness 5 mm) and a donut-shaped glass filter plate {diameter 60 mm, inner diameter 30 mm, thickness 5 mm; liquid discharge part (30)} Providing a cylindrical bottom (40) configured;
Further, a hard vinyl chloride funnel member (open portion inner diameter 30 mm, thickness 5 mm, height 30 mm) is provided 10 mm lower end open side from the circular bottom portion (40) to create a circular container (50) (FIGS. 7 to 9). ).
On the other hand, at the lower end of a rigid vinyl chloride cylinder {inner diameter 20 mm, length 50 mm, thickness 5 mm (up to 20 mm from the lower end of the cylinder) and thickness 14.5 mm (up to 30 mm from the upper end of the cylinder)}. Four circular holes with a diameter of 5 mm {liquid discharge part (60)} are provided at equal intervals so as to be in contact with each other. Further, 10 mm above the liquid discharge part (60) inside the hard vinyl chloride cylinder is made of hard vinyl chloride. A cylindrical part (70) provided with an umbrella-shaped member (110) made of a donut-shaped ring (ring width 3 mm, outer peripheral side thickness 5 mm, inner week side thickness 3 mm);
A Teflon donut ring with a disk member {diameter 55 mm, thickness in contact with the cylindrical portion (70) 8 mm, outer peripheral thickness 3 mm} made from a wire mesh (JIS Z8801-1; 2000) with 150 μm mesh A piston (90) was created from a filter medium part (80) provided with a sliding member (120) composed of (diameter 59 mm, inner diameter 55 mm, thickness 3 mm) (FIGS. 7 and 10 to 11).
The cylindrical container (50) is erected so that the cylindrical axis is in the vertical direction (gravity axis direction), and the piston (90) is inserted into the cylindrical container (50). A rigid vinyl chloride cylindrical container (inner diameter: 45 mm, thickness: 5 mm) {container for receiving the liquid flowing out from the liquid discharge part (30)} with the lower end open portion closed at 55 mm (thickness: 5 mm) is disposed below the funnel member By doing (FIG. 7), the liquid absorption performance measuring apparatus (AME2) of this invention was created.
Table 1 shows the average value of the liquid amount (W10) in the same manner as in Example 1 except that the device <AME-1> was changed to the device <AME-2>.

<Comparative Example 1>
For the measurement samples (1) to (15) obtained in Example 1, the average amount of water absorption using saline in accordance with JIS K7223-1996 {Water absorption test method of superabsorbent resin; teabag method}. Values were determined and shown in Table 1.

<Comparative example 2>
For the measurement samples (1) to (15) obtained in Example 1, the amount of liquid was measured in accordance with the description in Example 1 of Patent Document 1. And these operations were repeated 5 times and the average value of 5 times was shown in Table 1.

<Comparative Example 3>
Table 1 shows the average value of the amount of water absorbed in the same manner as in Comparative Example 1 except that the saline was changed to artificial urine.

<Comparative example 4>
The amount of liquid was measured in the same manner as in Comparative Example 2 except that the donut weight (0.20 Kg) was changed to a donut weight (0.50 Kg). And these operations were repeated 5 times and the average value of 5 times was shown in Table 1.

<Comparative Example 5>
The amount of liquid was measured in the same manner as in Comparative Example 2 except that the physiological saline flow rate was changed from 10 ml / min to 20 ml / min. And these operations were repeated 5 times and the average value of 5 times was shown in Table 1.

<Comparative Example 6>
Minerals whose liquid-absorbing particles (A1) to (A15) were changed to Uremer (urea resin manufactured by Meito Chemical Co., Ltd.) and whose kinematic viscosity (m ² / s) at 40 ° C. was 5 × 10 ⁻⁶ The amount of liquid was measured in the same manner as in Comparative Example 2 except that it was changed to oil. And these operations were repeated 5 times and the average value of 5 times was shown in Table 1.

<Evaluation in actual use>
Based on the description of <Production Example 1> to <Comparative Production Example 3> in Patent Document 1, paper diapers (1) to (15) were prepared.
For these disposable diapers (1) to (15), the “absorption amount until leakage” and the “surface dryness value by SDME” were measured based on the description of evaluation of actual use in Patent Document 1 (paragraphs 0195 to 0198). . And these operations were repeated 5 times and the average value of 5 times was shown in Table 1.
Further, the “surface dry feeling” of the paper diapers (1) to (15) was evaluated as shown in Table 1.

<Dry surface>
Using the paper diaper after the amount of absorption until leakage was measured, the dry feeling of the surface of the paper diaper was determined by touching with 10 panelists and quantified as follows. The average value of 10 people was obtained and shown in Table 1.
Good dry feeling: 3 points Slightly damp, but satisfactory level of dry feeling: 2 points Poor dry feeling, wet or no dry feeling, wet condition: 1 point

  The relationship between “absorption amount until leakage” or “surface dryness value” and measured values of Examples 1 to 10 or Comparative Examples 1 to 5 is shown in FIGS. Further, the correlation coefficient was obtained with MicroSoft EXCEL (a spreadsheet software of Microsoft Corporation) and shown in Table 2.

  From Tables 1 and 2 and FIGS. 15 to 20, the measured values of Examples 1 to 10 are more absorbable in actual use (paper diapers) than the measured values of Comparative Examples 1 to 5 (absorption amount until leakage, surface dryness). It was found that the correlation with the feeling and surface dryness value was extremely high.

It is front sectional drawing which showed typically the whole one Embodiment (Example 1) of the measuring apparatus of this invention. It is the top view which showed typically the cylindrical container (50) used for one Embodiment (Example 1) of the measuring apparatus of this invention. It is the side view which showed typically the cylindrical container (50) used for one Embodiment (Example 1) of the measuring apparatus of this invention. It is the top view which showed typically the piston (90) used for one Embodiment (Example 1) of the measuring apparatus of this invention. It is the side view which showed typically the piston (90) used for one Embodiment (Example 1) of the measuring apparatus of this invention. It is the reverse view which showed typically the piston (90) used for one Embodiment (Example 1) of the measuring apparatus of this invention. It is front sectional drawing which showed typically the whole one Embodiment (Example 11) of the measuring apparatus of this invention. It is the side view which showed typically the cylindrical container (50) used for one Embodiment (Example 11) of the measuring apparatus of this invention. It is the reverse view which showed typically the cylindrical container (50) used for one Embodiment (Example 11) of the measuring apparatus of this invention. It is the top view which showed typically the piston (90) used for one Embodiment (Example 11) of the measuring apparatus of this invention. It is the side view which showed typically the piston (90) used for one Embodiment (Example 11) of the measuring apparatus of this invention. It is the top view which showed typically the piston (90) used for one Embodiment of the measuring apparatus of this invention. It is the upper surface which showed typically the piston (90) used for one Embodiment of the measuring apparatus of this invention. It is front sectional drawing which showed typically the piston (90) used for one Embodiment of the measuring apparatus of this invention. It is a graph showing the relationship between the “absorption amount until leakage” and the measured values of Examples 1 to 4 and Comparative Example 1. It is a graph showing the relationship between the “absorption amount until leakage” and measured values of Examples 5 to 7 and Comparative Examples 2 and 3. 6 is a graph showing the relationship between “absorption amount until leakage” and measured values of Examples 8, 9, 11 and Comparative Examples 4, 5. 4 is a graph showing the relationship between “surface dryness value” and measured values of Examples 1 to 4 and Comparative Example 1. It is a graph showing the relationship between "surface dryness value" and the measured values of Examples 5 to 7 and Comparative Examples 2 and 3. It is a graph showing the relationship between the “surface dryness value” and measured values of Examples 8, 9, 11 and Comparative Examples 4 and 5.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Liquid discharge port 20 Cylindrical part 30 Liquid discharge port 40 Circular bottom part 50 Cylindrical container 60 Liquid discharge port 70 Cylindrical part 80 Filter medium part 90 Piston 100 Liquid injection port 110 Umbrella-shaped member 120 Sliding member

Claims (7)

A cylindrical container (50) comprising a cylindrical part (20) having a liquid discharge port (10) and a circular bottom part (40) having a liquid discharge part (30) at least on the outer peripheral part is erected so that the cylindrical axis is vertical. After putting the measurement sample into this cylindrical container (50),
A piston (90) composed of a cylindrical part (70) having a liquid discharge part (60) and a filter medium part (80) is inserted into the cylindrical container (50), and a liquid inlet at the top of the cylindrical part (70) is inserted. Inject liquid from (100)
The amount of liquid injected before the liquid flows out from the liquid outlet (10) and / or the liquid outlet (30); and / or the liquid flowing out from the liquid outlet (10) and / or the liquid outlet (30) A method for measuring liquid absorption performance, characterized by measuring the amount of water. The measurement method according to claim 1, wherein the measurement is performed by applying a weight to the measurement sample via the piston (90). The measurement method according to claim 1 or 2, wherein the measurement sample is prepared by uniformly mixing the liquid-absorbing particles (A) and the fine particles (B) having a weight average particle diameter of 100 to 700 µm. The measurement method according to claim 3, wherein the fine particles (B) are shirasu balloons. The content of (A) is 10 to 90% by weight and the content of (B) is 10 to 90% by weight based on the weight of the liquid-absorbing particles (A) and the fine particles (B). The measuring method as described in. An apparatus for measuring the liquid absorption performance of liquid absorbent particles,
A cylindrical container (50) comprising a cylindrical part (20) having a liquid discharge port (10) and a circular bottom part (40) having a liquid discharge part (30) at least on the outer periphery;
A piston (90) comprising a cylindrical part (70) having a liquid discharge part (60) and a liquid inlet (100), and a filter medium part (80);
A liquid absorption performance measuring device characterized by comprising: The liquid absorption according to claim 6, wherein the ratio (S1 / S2) of the ratio of the cross-sectional area (S1) of the liquid discharge part (30) and the cross-sectional area (S2) of the liquid inlet (100) is 2 to 10,000. Performance measuring device.

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