WO2021039714A1 - Absorbent article and auxiliary sheet - Google Patents
Absorbent article and auxiliary sheet Download PDFInfo
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- WO2021039714A1 WO2021039714A1 PCT/JP2020/031838 JP2020031838W WO2021039714A1 WO 2021039714 A1 WO2021039714 A1 WO 2021039714A1 JP 2020031838 W JP2020031838 W JP 2020031838W WO 2021039714 A1 WO2021039714 A1 WO 2021039714A1
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- water
- resin particles
- absorbent resin
- liquid
- sheet
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/45—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the shape
- A61F13/49—Absorbent articles specially adapted to be worn around the waist, e.g. diapers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
- A61F13/534—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having an inhomogeneous composition through the thickness of the pad
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F2013/15008—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterized by the use
- A61F2013/15146—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterized by the use for urine collection
Definitions
- the present invention relates to an absorbent article and an auxiliary sheet.
- Absorbents containing water-absorbent resin particles are generally used as absorbent articles for absorbing water-based liquids such as urine.
- water-absorbent sheet structure disclosed in Patent Document 1 below water-absorbent resin particles having a physiological saline water absorption rate within a predetermined range are used in the liquid-absorbent layer.
- one aspect of the present invention is to provide an absorbent article in which liquid leakage at the initial stage of liquid absorption is suppressed.
- Another aspect of the present invention is to provide an auxiliary sheet capable of suppressing liquid leakage in the initial stage of liquid absorption in an absorbent article.
- One aspect of the present invention includes a water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet and a liquid permeable sheet, and includes a liquid impermeable sheet, an auxiliary sheet, a water absorbing core and a liquid permeable sheet.
- the auxiliary sheet includes a resin layer containing water-absorbent resin particles, and the following steps (1), (2), (3), (4) and (5) are included in this order.
- the measured dry powder passing liquid absorption rate of the water-absorbent resin particles is 0.25 or more and 1.0 or less.
- 0.2 g of water-absorbent resin particles are uniformly sprayed over the entire bottom surface of a cylindrical container having an inner diameter of 60 mm having a mesh-like bottom, and the total amount of the container and the water-absorbent resin particles sprayed in the container.
- the mass Wb (g) is measured.
- 20 mL of artificial urine having a liquid temperature of 25 ° C. is injected into the container on which the water-absorbent resin particles are sprayed at a constant rate of 8 mL / sec, and at least a part of the artificial urine is absorbed by the water-absorbent resin particles to make the container.
- a swelling gel is formed within.
- the dry powder passing liquid absorption amount (g) is determined from Wa (g) -Wb (g).
- the dry powder passage liquid absorption rate (g / g) is obtained as the ratio of the dry powder passage liquid absorption amount (g) to the artificial urine saturated liquid absorption amount (g) of 0.2 g of the water-absorbent resin particles.
- an auxiliary sheet capable of suppressing liquid leakage in the initial stage of liquid absorption in an absorbent article.
- each component in the composition means the total amount of the plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified.
- the absorbent article according to the embodiment includes a water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet, and a liquid permeable sheet.
- the liquid impermeable sheet, the auxiliary sheet, the water absorbing core and the liquid permeable sheet are arranged in this order. That is, the auxiliary sheet is arranged so as to be in contact with the surface of the absorbent core provided with the water absorbing core, which is opposite to the side on which the liquid to be absorbed is invaded.
- the auxiliary sheet is used in an absorbent article provided with a water absorbing core to assist the liquid absorption of the water absorbing core.
- the auxiliary sheet includes a resin layer containing water-absorbent resin particles, and is measured by a method including the following steps (1), (2), (3), (4) and (5) in this order.
- the dry powder water absorption rate of the resin particles is 0.25 or more and 1.0 or less.
- (1) 0.2 g of water-absorbent resin particles are uniformly sprayed over the entire bottom surface of a cylindrical container having an inner diameter of 60 mm having a mesh-like bottom, and the total amount of the container and the water-absorbent resin particles sprayed in the container.
- the mass Wb (g) is measured.
- the dry powder passing liquid absorption amount (g) is determined from Wa (g) -Wb (g).
- the dry powder passage liquid absorption rate (g / g) is obtained as the ratio of the dry powder passage liquid absorption amount (g) to the artificial urine saturated liquid absorption amount (g) of 0.2 g of the water-absorbent resin particles.
- the artificial urine sodium chloride (NaCl) 100.0 g, calcium chloride dihydrate (CaCl 2 ⁇ H 2 O) 3.0g, magnesium chloride hexahydrate (MgCl 2 ⁇ 6H 2 O) It is an aqueous solution prepared from 6.0 g, 25.0 g of Triton X-100 (1%), 0.25 g of Edible Blue No. 1, and 9865.75 g of water.
- the artificial urine saturated liquid absorption amount is an index showing the saturated liquid absorption amount of artificial urine in a predetermined amount of water-absorbent resin particles, and the dry powder passing liquid absorption amount is a short time after contact between the water-absorbent resin particles and artificial urine. It is an index that reflects the amount of liquid absorbed during (initial).
- the high dry powder passage liquid absorption rate which is the ratio of the dry powder passage liquid absorption amount to the artificial urine saturated liquid absorption amount, means that the liquid permeability of the water-absorbent resin particles in a short time (initial) after contact with artificial urine is high. It is thought to mean high.
- the auxiliary sheet provided with the resin layer containing the water-absorbent resin particles having high liquid permeability at the initial stage instantly absorbs the liquid that could not be absorbed by the water-absorbing core, so that the liquid at the initial stage of liquid absorption in the absorbent article It is presumed that leakage will be suppressed.
- the lower limit of the liquid absorption rate of dry powder is 0.25 or more, and from the viewpoint of further excellent effect of suppressing liquid leakage in the initial stage of liquid absorption, 0.30 or more, 0.35 or more, 0.40 or more, 0. It may be 45 or more, 0.50 or more, 0.55 or more, 0.60 or more, 0.65 or more, 0.70 or more, 0.75 or more, 0.80 or more, or 0.85 or more.
- the upper limit of the dry powder passing liquid absorption rate is 1.0 or less, and may be 0.95 or less, or 0.90 or less.
- the artificial urine saturated liquid absorption amount of 0.2 g of the water-absorbent resin particles shows the same amount of saturated absorption of 0.2 g of the water-absorbent resin particles as the amount used for measuring the dry powder passage liquid absorption rate, and therefore is usually the same amount.
- the upper limit of the dry powder liquid absorption rate is usually 1.0 or less.
- the amount of dry powder flowing through is, for example, 2.7 g or more, 3.0 g or more, 4.0 g or more, 5.0 g or more, 6.0 g or more, 7.0 g or more, 8.0 g or more, or 9.0 g or more. It may be 15.0 g or less, 12.0 g or less, or 10.0 g or less.
- a specific method for measuring the amount of dry powder flowing through the liquid is as described in Examples described later.
- the artificial urine saturated liquid absorption amount of 0.2 g of the water-absorbent resin particles is calculated by a method including the following steps (a), (b), (c), (d) and (e) in this order.
- (A) Put 500 g of artificial urine into a 500 mL beaker.
- (B) 2.0 g of water-absorbent resin particles are charged into the beaker into which the artificial urine is charged while stirring the artificial urine at 600 rpm using a magnetic stirrer bar (8 mm ⁇ ⁇ 30 mm, without ring).
- C The artificial urine and the water-absorbent resin particles are stirred at 600 rpm for 60 minutes after the water-absorbent resin particles are added to form a swollen gel.
- the artificial urine saturated liquid absorption amount of 0.2 g of the water-absorbent resin particles is, for example, 7.0 or more, 8.0 or more, 9.0 or more, or 10.0 from the viewpoint of the water absorption characteristics of the water-absorbent resin particles. It may be 20.0 or less, 15.0 or less, 13.0 or less, or 11.0 or less.
- a specific method for measuring the artificial urine saturated liquid absorption amount of 0.2 g of the water-absorbent resin particles is as described in Examples described later.
- the shape of the water-absorbent resin particles may be, for example, substantially spherical, crushed or granular, and particles having agglomerated primary particles having these shapes may be formed.
- the medium particle size of the water-absorbent resin particles may be 45 to 850 ⁇ m, 75 to 700 ⁇ m, 100 to 600 ⁇ m, or 200 to 600 ⁇ m.
- the water-absorbent resin particles may have a desired particle size distribution at the time of being obtained by the production method described later, but the particle size distribution may be adjusted by performing an operation such as particle size adjustment using classification with a sieve. Good.
- the water-absorbent resin particles can include, for example, a crosslinked polymer formed by polymerizing a monomer containing an ethylenically unsaturated monomer.
- the crosslinked polymer has a monomer unit derived from an ethylenically unsaturated monomer.
- the water-absorbent resin particles can be produced by a method including a step of polymerizing a monomer containing an ethylenically unsaturated monomer.
- the polymerization method include a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method. From the viewpoint of ensuring good water absorption characteristics of the obtained water-absorbent resin particles and facilitating control of the polymerization reaction, a reverse phase suspension polymerization method or an aqueous solution polymerization method may be applied. In the following, a reverse phase suspension polymerization method will be described as an example as a method for polymerizing an ethylenically unsaturated monomer.
- the ethylenically unsaturated monomer may be water-soluble.
- water-soluble ethylenically unsaturated monomers include (meth) acrylic acid and its salts, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts, (meth) acrylamide, N, N-dimethyl.
- the ethylenically unsaturated monomer has an amino group, the amino group may be quaternized.
- the ethylenically unsaturated monomer may be used alone or in combination of two or more.
- Functional groups such as the carboxyl group and amino group of the above-mentioned monomers can function as functional groups capable of cross-linking in the surface cross-linking step described later.
- the ethylenically unsaturated monomer is at least one selected from the group consisting of (meth) acrylic acid and salts thereof, acrylamide, methacrylamide, and N, N-dimethylacrylamide. It may contain a compound of the species.
- the ethylenically unsaturated monomer may contain (meth) acrylic acid and a salt thereof, and at least one compound selected from the group consisting of acrylamide.
- the ethylenically unsaturated monomer may contain at least one compound selected from the group consisting of (meth) acrylic acid and salts thereof.
- the ethylenically unsaturated monomer can be used in the polymerization reaction as an aqueous solution.
- concentration of the ethylenically unsaturated monomer in the aqueous solution containing the ethylenically unsaturated monomer (hereinafter, simply referred to as "monomer aqueous solution") is 20% by mass or more and the saturation concentration or less, 25 to 70% by mass, or 30. It may be up to 55% by mass.
- Examples of the water used in the aqueous solution include tap water, distilled water, ion-exchanged water and the like.
- a monomer other than the above-mentioned ethylenically unsaturated monomer may be used.
- Such a monomer can be used, for example, by being mixed with an aqueous solution containing the above-mentioned ethylenically unsaturated monomer.
- the amount of the ethylenically unsaturated monomer used may be 70 to 100 mol% with respect to the total amount of the monomers.
- the ratio of (meth) acrylic acid and a salt thereof may be 70 to 100 mol% with respect to the total amount of the monomer.
- the acid group may be neutralized with an alkaline neutralizer and then the monomer solution may be used in the polymerization reaction.
- the degree of neutralization of an ethylenically unsaturated monomer by an alkaline neutralizing agent increases the osmotic pressure of the obtained water-absorbent resin particles and further enhances the water absorption characteristics (water absorption amount, etc.). It may be 10-100 mol%, 50-90 mol%, or 60-80 mol% of the acidic group in the body.
- the alkaline neutralizer include alkali metal salts such as sodium hydroxide, sodium carbonate, sodium hydrogen carbonate, potassium hydroxide and potassium carbonate; ammonia and the like.
- the alkaline neutralizer may be used alone or in combination of two or more.
- the alkaline neutralizer may be used in the form of an aqueous solution to simplify the neutralization operation.
- Neutralization of the acid group of the ethylenically unsaturated monomer can be performed, for example, by adding an aqueous solution of sodium hydroxide, potassium hydroxide or the like to the above-mentioned monomer aqueous solution and mixing them.
- the monomer aqueous solution is dispersed in a hydrocarbon dispersion medium in the presence of a surfactant, and the ethylenically unsaturated monomer is polymerized using a radical polymerization initiator or the like.
- a radical polymerization initiator a water-soluble radical polymerization initiator can be used.
- surfactant examples include nonionic surfactants and anionic surfactants.
- nonionic surfactant sorbitan fatty acid ester and (poly) glycerin fatty acid ester (“(poly)” means both with and without the prefix of “poly”. The same shall apply hereinafter.
- Sucrose fatty acid ester polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, sorbitol fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene himashi
- oil polyoxyethylene cured castor oil, alkylallyl formaldehyde condensed polyoxyethylene ether, polyoxyethylene polyoxypropylene block copolymer, polyoxyethylene polyoxypropyl alkyl ether, polyethylene glycol fatty acid ester and the like.
- anionic surfactants include fatty acid salts, alkylbenzene sulfonates, alkylmethyl taurates, polyoxyethylene alkylphenyl ether sulfates, polyoxyethylene alkyl ether sulfonates, and phosphoric acid esters of polyoxyethylene alkyl ethers. , And the phosphate ester of polyoxyethylene alkyl allyl ether and the like.
- the surfactant may be used alone or in combination of two or more.
- the surfactant is a sorbitan fatty acid ester. It may contain at least one compound selected from the group consisting of polyglycerin fatty acid ester and sucrose fatty acid ester. From the viewpoint of easily improving the water absorption characteristics of the obtained water-absorbent resin particles, a sorbitan fatty acid ester and / or a sucrose fatty acid ester (for example, sucrose stearic acid ester) can be used as the surfactant. These surfactants may be used alone or in combination of two or more.
- the amount of the surfactant may be 0.05 to 10 parts by mass, 0.08 to 5 parts by mass, or 0.1 to 3 parts by mass with respect to 100 parts by mass of the monomer aqueous solution.
- a polymer-based dispersant may be used in combination with the above-mentioned surfactant.
- the polymer dispersant include maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, maleic anhydride-modified ethylene / propylene copolymer, maleic anhydride-modified EPDM (ethylene / propylene / diene / terpolymer), and maleic anhydride.
- the polymer-based dispersant may be used alone or in combination of two or more.
- the polymer-based dispersant includes maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, maleic anhydride-modified ethylene / propylene copolymer, and maleic anhydride / ethylene copolymer.
- Maleic anhydride / propylene copolymer, maleic anhydride / ethylene / propylene copolymer, polyethylene, polypropylene, ethylene / propylene copolymer, oxidized polyethylene, oxidized polypropylene, and oxidized ethylene / propylene copolymer It may be at least one selected from the group consisting of.
- the amount of the polymer-based dispersant may be 0.05 to 10 parts by mass, 0.08 to 5 parts by mass, or 0.1 to 3 parts by mass with respect to 100 parts by mass of the monomer aqueous solution.
- the hydrocarbon dispersion medium may contain at least one compound selected from the group consisting of chain aliphatic hydrocarbons having 6 to 8 carbon atoms and alicyclic hydrocarbons having 6 to 8 carbon atoms.
- Hydrocarbon dispersion media include chain aliphatic hydrocarbons such as n-hexane, n-heptane, 2-methylhexane, 3-methylhexane, 2,3-dimethylpentane, 3-ethylpentane, and n-octane; cyclohexane.
- the hydrocarbon dispersion medium may be used alone or in combination of two or more.
- the hydrocarbon dispersion medium may contain at least one selected from the group consisting of n-heptane and cyclohexane.
- the mixture of the above-mentioned hydrocarbon dispersion medium for example, commercially available ExxonHeptane (manufactured by ExxonMobil: containing 75 to 85% of n-heptane and isomeric hydrocarbons) is used. You may.
- the amount of the hydrocarbon dispersion medium is 30 to 1000 parts by mass, 40 to 500 parts by mass, or 50 parts by mass with respect to 100 parts by mass of the monomer aqueous solution from the viewpoint of appropriately removing the heat of polymerization and easily controlling the polymerization temperature. It may be up to 300 parts by mass. When the amount of the hydrocarbon dispersion medium is 30 parts by mass or more, the polymerization temperature tends to be easily controlled. When the amount of the hydrocarbon dispersion medium is 1000 parts by mass or less, the productivity of polymerization tends to be improved, which is economical.
- the radical polymerization initiator may be water-soluble.
- water-soluble radical polymerization initiators are persulfates such as potassium persulfate, ammonium persulfate, and sodium persulfate; methyl ethyl ketone peroxide, methyl isobutyl ketone peroxide, di-t-butyl peroxide, and t-butyl cumylper.
- Peroxides such as oxides, t-butylperoxyacetate, t-butylperoxyisobutyrate, t-butylperoxypivalate, hydrogen peroxide; 2,2'-azobis (2-amidinopropane) dihydrochloride , 2,2'-azobis [2- (N-phenylamidino) propane] dihydrochloride, 2,2'-azobis [2- (N-allylamidino) propane] dihydrochloride, 2,2'-azobis [ 2- (2-Imidazolin-2-yl) propane] 2 hydrochloride, 2,2'-azobis ⁇ 2- [1- (2-hydroxyethyl) -2-imidazolin-2-yl] propane ⁇ 2 hydrochloride, 2,2'-azobis ⁇ 2-methyl-N- [1,1-bis (hydroxymethyl) -2-hydroxyethyl] propionamide ⁇ , 2,2'-azobis [2-methyl-N- (2-hydroxy) Ethyl) -propion
- the radical polymerization initiator may be used alone or in combination of two or more.
- the radical polymerization initiators are potassium persulfate, ammonium persulfate, sodium persulfate, 2,2'-azobis (2-amidinopropane) dihydrochloride, 2,2'-azobis [2- (2-imidazolin-2-yl). ) Propane] 2 hydrochloride and 2,2'-azobis ⁇ 2- [1- (2-hydroxyethyl) -2-imidazolin-2-yl] propane ⁇ 2 hydrochloride at least selected from the group. There may be.
- the amount of the radical polymerization initiator may be 0.00005 to 0.01 mol per 1 mol of the ethylenically unsaturated monomer.
- the amount of the radical polymerization initiator used is 0.00005 mol or more, the polymerization reaction does not require a long time and is efficient.
- the amount of the radical polymerization initiator is 0.01 mol or less, it is easy to suppress the occurrence of a rapid polymerization reaction.
- the exemplified radical polymerization initiator can also be used as a redox polymerization initiator in combination with a reducing agent such as sodium sulfite, sodium hydrogen sulfite, ferrous sulfate, and L-ascorbic acid.
- a reducing agent such as sodium sulfite, sodium hydrogen sulfite, ferrous sulfate, and L-ascorbic acid.
- the aqueous monomer solution may contain a chain transfer agent.
- chain transfer agent include hypophosphates, thiols, thiolic acids, secondary alcohols, amines and the like.
- the monomer aqueous solution used for the polymerization may contain a thickener.
- the thickener include hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, carboxymethyl cellulose, polyacrylic acid, polyethylene glycol, polyacrylamide, polyethyleneimine, dextrin, sodium alginate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide and the like. If the stirring speed at the time of polymerization is the same, the higher the viscosity of the aqueous monomer solution, the larger the medium particle size of the obtained particles tends to be.
- Cross-linking by self-cross-linking may occur during polymerization, but cross-linking may be further performed by using an internal cross-linking agent.
- an internal cross-linking agent When an internal cross-linking agent is used, it is easy to control the water absorption characteristics of the water-absorbent resin particles.
- the internal cross-linking agent is usually added to the reaction solution during the polymerization reaction.
- the internal cross-linking agent examples include di or tri (meth) acrylic acid esters of polyols such as ethylene glycol, propylene glycol, trimethylpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; Unsaturated polyesters obtained by reacting polyols with unsaturated acids (maleic acid, fumaric acid, etc.); bis (meth) acrylamides such as N, N'-methylenebis (meth) acrylamide; polyepoxides and (meth) Di or tri (meth) acrylic acid esters obtained by reacting with acrylic acid; di (meth) obtained by reacting polyisocyanate (tolylene diisocyanate, hexamethylene diisocyanate, etc.) with hydroxyethyl (meth) acrylate.
- polyols such as ethylene glycol, propylene glycol, trimethylpropane, glycerin, polyoxyethylene glycol, polyoxypropy
- Acrylic acid carbamil esters compounds having two or more polymerizable unsaturated groups, such as allylated starch, allylated cellulose, diallyl phthalate, N, N', N "-triallyl isocyanurate, divinylbenzene; Poly such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, polyglycerol polyglycidyl ether, etc.
- Poly such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propy
- Glyceridyl compound such as epichlorohydrin, epibromhydrin, ⁇ -methylepichlorohydrin; 2 reactive functional groups such as isocyanate compound (2,4-tolylene diisocyanate, hexamethylene diisocyanate, etc.) Examples thereof include compounds having more than one.
- the internal cross-linking agent may be used alone or in combination of two or more.
- the internal cross-linking agent may be a polyglycidyl compound or diglycidyl. It may be an ether compound.
- the internal cross-linking agent comprises at least one selected from the group consisting of (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, and (poly) glycerin diglycidyl ether. It may be.
- the amount of the internal cross-linking agent is not ethylenious from the viewpoint that the water-soluble property is suppressed by appropriately cross-linking the polymer obtained by the polymerization of the above-mentioned monomer aqueous solution, and a sufficient water absorption amount can be easily obtained. It may be 0 mmol or more, 0.01 mmol or more, 0.015 mmol or more, 0.020 mmol or more, or 0.1 mol or less, per 1 mol of saturated monomer.
- Reverse-phase suspension polymerization can be carried out in an aqueous system in oil by heating with stirring in a state where the phases are mixed.
- a monomer aqueous solution containing an ethylenically unsaturated monomer is used as a hydrocarbon dispersion medium in the presence of a surfactant (and, if necessary, a polymer-based dispersant). Disperse in.
- a surfactant and, if necessary, a polymer-based dispersant.
- the timing of adding the surfactant, the polymer-based dispersant, etc. may be either before or after the addition of the monomer aqueous solution.
- the monomer aqueous solution is dispersed in the hydrocarbon dispersion medium in which the polymer-based dispersant is dispersed, and then the surfactant is further dispersed. It may be allowed to carry out polymerization.
- Reverse phase suspension polymerization can be carried out in one stage or in multiple stages of two or more stages. Reversed phase suspension polymerization may be carried out in two or three stages from the viewpoint of increasing productivity.
- an ethylenically unsaturated monomer is added to the reaction mixture obtained in the first step polymerization reaction after the first step reverse phase suspension polymerization is carried out. It may be added and mixed, and the reverse phase suspension polymerization of the second and subsequent steps may be carried out in the same manner as in the first step.
- the above-mentioned radical polymerization initiator is used in the reverse phase suspension polymerization in each stage of the second and subsequent stages.
- the ethylenically unsaturated monomer to be added Based on the amount of the ethylenically unsaturated monomer to be added, it may be added within the range of the molar ratio of each component to the above-mentioned ethylenically unsaturated monomer to carry out reverse phase suspension polymerization.
- an internal cross-linking agent In the reverse phase suspension polymerization in each stage after the second stage, an internal cross-linking agent may be used if necessary.
- an internal cross-linking agent When an internal cross-linking agent is used, it is added within the range of the molar ratio of each component to the above-mentioned ethylenically unsaturated monomer based on the amount of the ethylenically unsaturated monomer provided in each stage, and the suspension is reversed. Muddy polymerization may be carried out.
- the temperature of the polymerization reaction varies depending on the radical polymerization initiator used, but by advancing the polymerization rapidly and shortening the polymerization time, the efficiency is improved and the heat of polymerization is easily removed to carry out the reaction smoothly. From the viewpoint, it may be 20 to 150 ° C. or 40 to 120 ° C.
- the reaction time is usually 0.5-4 hours.
- the completion of the polymerization reaction can be confirmed, for example, by stopping the temperature rise in the reaction system. As a result, the polymer of the ethylenically unsaturated monomer is usually obtained in the state of a hydrogel-like polymer.
- cross-linking may be performed after polymerization by adding a cross-linking agent to the obtained hydrogel polymer and heating it.
- a cross-linking agent to the obtained hydrogel polymer and heating it.
- cross-linking agent for performing post-polymerization cross-linking examples include polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; Compounds having two or more epoxy groups such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, and (poly) glycerin diglycidyl ether; epichlorohydrin, epibromhydrin, ⁇ -methylepicrolhydrin, etc.
- polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane
- glycerin polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin
- Compounds having two or more epoxy groups such as (poly) ethylene glycol
- Haloepoxide compounds compounds having two or more isocyanate groups such as 2,4-tolylene diisocyanate and hexamethylene diisocyanate; oxazoline compounds such as 1,2-ethylenebisoxazoline; carbonate compounds such as ethylenecarbonate; bis [N , N-di ( ⁇ -hydroxyethyl)] hydroxyalkylamide compounds such as adipamide can be mentioned.
- Cross-linking agents for post-polymerization cross-linking are (poly) ethylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, and polyglycerol polyglycidyl ether. It may be a polyglycidyl compound such as. These cross-linking agents may be used alone or in combination of two or more.
- the amount of the cross-linking agent used for post-polymerization cross-linking is 1 mol of the water-soluble ethylenically unsaturated monomer from the viewpoint of appropriately cross-linking the obtained hydrogel-like polymer to exhibit suitable water absorption characteristics. It may be 0 to 0.03 mol, 0 to 0.01 mol, or 0.00001 to 0.005 mol.
- the cross-linking agent for post-polymerization cross-linking is added to the reaction solution after the polymerization reaction of the ethylenically unsaturated monomer.
- a cross-linking agent for post-polymerization cross-linking may be added after the multi-stage polymerization.
- the cross-linking agent for post-polymerization cross-linking is , From the viewpoint of water content (described later), it may be added in the region of [water content immediately after polymerization ⁇ 3% by mass].
- drying to remove water gives polymer particles containing a polymer of ethylenically unsaturated monomers.
- the drying method include (a) a method of removing water by azeotropic distillation in a state where the hydrogel polymer is dispersed in a hydrocarbon dispersion medium, and (b) a method of taking out the hydrogel polymer by decantation and reducing the pressure. Examples thereof include a method of drying, (c) a method of filtering the hydrogel polymer by a filter and drying under reduced pressure.
- the particle size of the water-absorbent resin particles can be adjusted by adjusting the rotation speed of the stirrer during the polymerization reaction, or by adding a flocculant into the system after the polymerization reaction or in the early stage of drying. By adding a flocculant, the particle size of the obtained water-absorbent resin particles can be increased.
- an inorganic flocculant can be used as the flocculant.
- the inorganic flocculant for example, powdered inorganic flocculant
- the aggregating agent may be at least one selected from the group consisting of silica, aluminum oxide, talc and kaolin.
- a coagulant is previously dispersed in a hydrocarbon dispersion medium of the same type as that used in the polymerization or water, and then this is placed in a hydrocarbon dispersion medium containing a hydrogel polymer under stirring. May be mixed with.
- the amount of the flocculant is 0.001 to 1 part by mass, 0.005 to 0.5 part by mass, or 0.01 to 0.2 with respect to 100 parts by mass of the ethylenically unsaturated monomer used for the polymerization. It may be a mass part. When the amount of the flocculant is within these ranges, it is easy to obtain water-absorbent resin particles having a desired particle size distribution.
- the polymerization reaction can be carried out using various stirrers having stirring blades.
- a flat plate blade a lattice blade, a paddle blade, a propeller blade, an anchor blade, a turbine blade, a Faudler blade, a ribbon blade, a full zone blade, a max blend blade and the like can be used.
- the flat plate blade has a shaft (stirring shaft) and a flat plate portion (stirring portion) arranged around the shaft. Further, the flat plate portion may have a slit or the like.
- the water content of the surface-crosslinked hydrogel polymer may be 5 to 50% by mass, 10 to 40% by mass, or 15 to 35% by mass.
- the amount of water in the hydrogel polymer calculated by adding the amount of water used as needed.
- Ws The amount of solids calculated from the amount of materials such as ethylenically unsaturated monomers, cross-linking agents, and initiators that make up the hydrogel polymer.
- cross-linking agents include polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; (poly) ethylene glycol diglycidyl.
- Polyglycidyl compounds such as ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, trimethylpropan triglycidyl ether (poly) propylene glycol polyglycidyl ether, (poly) glycerol polyglycidyl ether; epichlorohydrin , Epibrom hydrin, ⁇ -methyl epichlorohydrin and other haloepoxy compounds; 2,4-tolylene diisocyanate, hexamethylene diisocyanate and other isocyanate compounds; 3-methyl-3-oxetane methanol, 3-ethyl-3-oxetane Oxetane compounds such as methanol, 3-butyl-3-oxetane methanol, 3-methyl-3-oxetane ethanol, 3-ethyl-3-oxetane ethanol, 3-butyl-3-ox
- the surface cross-linking agent may be used alone or in combination of two or more.
- the surface cross-linking agent may be a polyglycidyl compound, and may be (poly) ethylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, and It may contain at least one selected from the group consisting of polyglycerol polyglycidyl ether.
- the amount of the surface cross-linking agent is 0.00001 to 0.02 mol, 0.00005 to 0.01 mol, or 0.0001 to 0.005 per 1 mol of the ethylenically unsaturated monomer used for the polymerization. It may be a molar.
- the amount of the surface cross-linking agent is 0.00001 mol or more, the cross-linking density on the surface portion of the water-absorbent resin particles is sufficiently increased, and the gel strength of the water-absorbent resin particles can be easily increased.
- the amount of the surface cross-linking agent is 0.02 mol or less, it is easy to increase the water absorption amount of the water-absorbent resin particles.
- the surface portion of the hydrogel polymer is treated (surface modification) with a surface modifier in either the drying step (moisture removal step) or a subsequent step. May be good.
- the surface modification may be carried out, for example, before, during or after the surface cross-linking step.
- Surface modification may be carried out after surface cross-linking.
- a hydrogel polymer obtained by a reverse phase suspension polymerization method, an aqueous solution polymerization method, or another polymerization method when the hydrogel polymer is treated with a surface modifier after surface cross-linking,
- the obtained water-absorbent resin particles tend to easily form a resin layer showing a high dry powder passing liquid absorption rate.
- the surface modifier may be, for example, a surfactant such as an anionic surfactant, a cationic surfactant, an amphoteric surfactant, or a nonionic surfactant.
- a surfactant such as an anionic surfactant, a cationic surfactant, an amphoteric surfactant, or a nonionic surfactant.
- the HLB value of the nonionic surfactant used as the surface modifier may be, for example, 3 to 12, or 6 to 10.
- the nonionic surfactant include sorbitan fatty acid esters such as sorbitan monolaurate.
- the surface modifier is a nonionic surfactant having an HLB value within the above range, the obtained water-absorbent resin particles tend to easily form a resin layer showing a high dry powder flow-through liquid absorption rate.
- the HLB value is measured by the Griffin method.
- the amount of the surface modifier is 0.01 to 0.50 parts by mass, 0.02 to 0.40 parts by mass, or 0.04 with respect to 100 parts by mass of the ethylenically unsaturated monomer used for the polymerization. It may be ⁇ 0.30 parts by mass.
- water and a hydrocarbon dispersion medium can be distilled off from the hydrogel polymer to obtain polymer particles which are dry products. it can.
- the water-absorbent resin particles according to the present embodiment may be composed of only polymer particles, but various additional particles selected from, for example, a gel stabilizer, a metal chelating agent, a fluidity improver (lubricant), and the like. Ingredients can be further included. Additional components may be placed inside the polymer particles, on the surface of the polymer particles, or both. The additional component may be a fluidity improver (lubricant).
- the fluidity improver may contain inorganic particles. Examples of the inorganic particles include silica particles such as amorphous silica.
- the water-absorbent resin particles may contain a plurality of inorganic particles arranged on the surface of the polymer particles. For example, by mixing the polymer particles and the inorganic particles, the inorganic particles can be arranged on the surface of the polymer particles.
- the inorganic particles may be silica particles such as amorphous silica.
- the ratio of the amount of the inorganic particles to the mass of the polymer particles is 0.2% by mass or more, 0.5% by mass or more, 1 It may be 0.0% by mass or more, 1.5% by mass or more, 5.0% by mass or less, or 3.5% by mass or less.
- the inorganic particles here usually have a minute size as compared with the size of the polymer particles.
- the average particle size of the inorganic particles may be 0.1 to 50 ⁇ m, 0.5 to 30 ⁇ m, or 1 to 20 ⁇ m.
- the average particle size here can be a value measured by a dynamic light scattering method or a laser diffraction / scattering method.
- FIG. 1 is a cross-sectional view showing an example of an auxiliary sheet.
- the auxiliary sheet 60 shown in FIG. 1 has a resin layer 61 and two sheet base materials 62a and 62b.
- the sheet base materials 62a and 62b are arranged on both sides of the resin layer 61.
- the resin layer 61 is arranged inside the sheet base materials 62a and 62b.
- the resin layer 61 is held in shape by being sandwiched between the two sheet base materials 62a and 62b.
- the sheet base materials 62a and 62b may be two sheets, one folded sheet, or one bag.
- the auxiliary sheet 60 may further have an adhesive 63a interposed between the sheet base material 62a and the resin layer 61, and further has an adhesive 63b interposed between the sheet base material 62b and the resin layer 61. You may have.
- the adhesives 63a and 63b may be, for example, a water-based adhesive, a solvent-based adhesive, an elastic adhesive, an aerosol adhesive, a hot melt adhesive, or the like.
- the thickness of the auxiliary sheet 60 may be, for example, 3.0 mm or less, 2.5 mm or less, 2.0 mm or less, or 1.8 mm or less, and 0.1 mm or more, 0.3 mm or more, or 0.5 mm or more. It may be.
- the thickness can be measured using, for example, a dial thickness gauge JB manufactured by Ozaki Seisakusho Co., Ltd. (the stylus is made of aluminum having a diameter of 50 mm).
- the resin layer 61 has the water-absorbent resin particles 61a according to the above-described embodiment and the fiber layer 61b containing a fibrous material.
- the resin layer 61 does not have to have the fiber layer 61b.
- the content of the water-absorbent resin particles in the resin layer may be 70 to 100% by mass, 80 to 100% by mass, or 90 to 100% by mass based on the mass of the resin layer 61.
- the thickness of the resin layer 61 may be, for example, 2.0 mm or less, 1.5 mm or less, 1.0 mm or less, or 0.8 mm or less in a dry state, and is 0.1 mm or more, or 0.3 mm or more. You may.
- the mass per unit area of the resin layer 61 may be 100 g / m 2 or less, 80 g / m 2 or less, 60 g / m 2 or less, or 40 g / m 2 or less, 10 g / m 2 or more, 20 g / m. It may be 2 or more, or 25 g / m 2 or more.
- the fibrous material constituting the fiber layer 61b can be, for example, a cellulosic fiber, a synthetic fiber, or a combination thereof.
- cellulosic fibers include crushed wood pulp, cotton, cotton linters, rayon and cellulosic acetate.
- synthetic fibers include polyamide fibers, polyester fibers, and polyolefin fibers.
- the fibrous material may be hydrophilic fibers (for example, pulp).
- the resin layer 61 may further contain inorganic particles (for example, amorphous silica), a deodorant, an antibacterial agent, a fragrance, and the like.
- the sheet base materials 62a and 62b may be, for example, non-woven fabric, tissue, or the like.
- the two sheet base materials 62a and 62b can be the same or different non-woven fabrics.
- the non-woven fabric may be a non-woven fabric composed of short fibers (that is, staples) (short-fiber non-woven fabric) or a non-woven fabric composed of long fibers (that is, filaments) (long-fiber non-woven fabric).
- the staples may generally have a fiber length of several hundred mm or less.
- the non-woven fabrics used as the sheet base materials 62a and 62b are thermal-bonded non-woven fabrics, air-through non-woven fabrics, resin-bonded non-woven fabrics, spunbonded non-woven fabrics, melt-blown non-woven fabrics, air-laid non-woven fabrics, spunlaced non-woven fabrics, point-bonded non-woven fabrics, or two or more kinds selected from these. It may be a laminate containing a non-woven fabric.
- the non-woven fabric used as the sheet base materials 62a and 62b can be a non-woven fabric formed of synthetic fibers, natural fibers, or a combination thereof.
- synthetic fibers include polyolefins such as polyethylene (PE) and polypropylene (PP), polyesters such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN), polyamides such as nylon, and Examples thereof include fibers containing a synthetic resin selected from rayon.
- Examples of natural fibers include fibers containing cotton, silk, hemp, or pulp (cellulose).
- the fibers forming the non-woven fabric may be polyolefin fibers, polyester fibers or a combination thereof.
- the sheet base materials 62a and 62b may be tissues.
- the tissues used as the sheet base materials 62a and 62b may be natural fibers or natural fibers mixed with synthetic fibers.
- the mass per unit area of the tissue may be 16 ⁇ 2 g / m 2.
- the thickness of the tissue may be 0.12 ⁇ 0.02 mm.
- the auxiliary sheet 60 can be obtained, for example, by sandwiching the resin layer 61 between the sheet base materials 62a and 62b and pressurizing the formed structure while heating it as necessary. If necessary, the adhesives 63a and 63b are arranged between the sheet base materials 62a and 62b and the resin layer 61.
- the auxiliary sheet 60 is used, for example, for producing various absorbent articles.
- absorbent articles include diapers (eg paper diapers), toilet training pants, incontinence pads, sanitary materials (sanitary napkins, tampons, etc.), sweat pads, pet sheets, toilet components, and animal waste treatment materials. Can be mentioned.
- FIG. 2 is a cross-sectional view showing an example of an absorbent article.
- the absorbent article 100 shown in FIG. 2 includes a water absorbing core 50, an auxiliary sheet 60, a liquid permeable sheet 30, and a liquid impermeable sheet 40.
- the water absorption core 50 and the auxiliary sheet 60 are sandwiched between the liquid permeable sheet 30 and the liquid impermeable sheet 40.
- the water absorption core 50 has an absorption layer 10 and two core wrap sheets 20a and 20b.
- the core wrap sheets 20a and 20b are arranged on both sides of the absorption layer 10.
- the absorbent layer 10 is arranged inside the core wrap sheets 20a and 20b, and is held in shape by being sandwiched between the two core wrap sheets.
- the core wrap sheets 20a and 20b may be separate sheets, one folded sheet, or one bag body.
- the water absorption core 50 does not have to have one or both of the two core wrap sheets 20a and 20b.
- the core wrap sheet 20a may not be arranged between the absorption layer 10 and the auxiliary sheet 60.
- the absorption layer 10 is sandwiched between one core wrap sheet 20b and the auxiliary sheet 60. It is kept in shape.
- the water absorption core 50 may further have an adhesive interposed between the core wrap sheet 20a and the absorption layer 10, and further has an adhesive interposed between the core wrap sheet 20b and the absorption layer 10. May be.
- An adhesive layer may be interposed between the core wrap sheets 20a and 20b on both sides and the absorption layer 10.
- FIG. 3 is a plan view showing an example of an adhesive application pattern formed on the core wrap sheet.
- the adhesive 21 shown in FIG. 3 forms a coating pattern composed of a plurality of linear portions arranged at intervals on the core wrap sheet 20a.
- the coating pattern of the adhesive 21 may be linear, curved, dot-shaped, or a combination thereof.
- the adhesive may be, for example, a water-based adhesive, a solvent-based adhesive, or a hot melt adhesive.
- the absorption layer 10 has water-absorbent resin particles 10a and a fiber layer 10b containing a fibrous material.
- the absorption layer 10 does not have to have the fiber layer 10b.
- the content of the water-absorbent resin particles in the absorption layer may be 70 to 100% by mass, 80 to 100% by mass, or 90 to 100% by mass based on the mass of the absorption layer 10.
- the water-absorbent resin particles 10a may be particles containing a polymer containing an ethylenically unsaturated monomer as a monomer unit.
- the ethylenically unsaturated monomer may be a water-soluble monomer, and examples thereof include (meth) acrylic acid and salts thereof, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts.
- the ethylenically unsaturated monomer may be used alone or in combination of two or more.
- the water-absorbent resin particles may be particles containing a polymer containing at least one of (meth) acrylic acid or a salt of (meth) acrylic acid as a monomer unit.
- the water-absorbent resin particles 10a can be produced, for example, by a method including polymerizing a monomer containing an ethylenically unsaturated monomer.
- the monomer polymerization method can be selected from, for example, a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method. From the viewpoint of ensuring good water absorption characteristics of the water-absorbent resin particles and easily controlling the polymerization reaction, a reverse phase suspension polymerization method or an aqueous solution polymerization method may be adopted.
- the polymer constituting the water-absorbent resin particles 10a may be a crosslinked polymer.
- the polymer may be crosslinked by self-crosslinking, cross-linking by reaction with a cross-linking agent, or both.
- the water-absorbent resin particles may be surface-crosslinked by cross-linking at least the polymer of the surface layer portion with a cross-linking agent.
- the water-absorbent resin particles 10a may contain various additional components in addition to the polymer of the ethylenically unsaturated monomer.
- additional ingredients include gel stabilizers, metal chelating agents, and fluidity improvers (lubricants).
- Additional components may be placed inside the polymer particles, including the polymer, on the surface of the polymer particles, or both.
- the additional component may be a fluidity improver (lubricant).
- the fluidity improver may contain inorganic particles. Examples of the inorganic particles include silica particles such as amorphous silica.
- the shape of the water-absorbent resin particles 10a may be, for example, substantially spherical, crushed or granular, and particles in which primary particles having these shapes are aggregated may be formed.
- the medium particle size of the water-absorbent resin particles may be 250 to 850 ⁇ m, 300 to 700 ⁇ m, or 300 to 600 ⁇ m.
- the water absorption amount of the physiological saline may be 20 to 80 g / g, 30 to 70 g / g, or 40 to 65 g / g.
- the thickness of the absorption layer 10 may be, for example, 20 mm or less, 15 mm or less, 10 mm or less, 5 mm or less, 4 mm or less, or 3 mm or less in a dry state, and may be 0.1 mm or more or 0.3 mm or more. Good.
- the mass per unit area of the absorption layer 10 may be 1000 g / m 2 or less, 800 g / m 2 or less, or 600 g / m 2 or less, 100 g / m 2 or more, or 200 g / m 2 or more. May be good.
- the fibrous material constituting the fiber layer 10b can be, for example, a cellulosic fiber, a synthetic fiber, or a combination thereof.
- cellulosic fibers include crushed wood pulp, cotton, cotton linters, rayon and cellulosic acetate.
- synthetic fibers include polyamide fibers, polyester fibers, and polyolefin fibers.
- the fibrous material may be hydrophilic fibers (for example, pulp).
- the absorption layer 10 may further contain an inorganic powder (for example, amorphous silica), a deodorant, an antibacterial agent, a fragrance, and the like.
- an inorganic powder for example, amorphous silica
- the absorption layer 10 may contain inorganic powder in addition to the inorganic particles in the water-absorbent resin particles 10a.
- the core wrap sheets 20a and 20b may be, for example, a non-woven fabric.
- the two core wrap sheets 20a and 20b can be the same or different non-woven fabrics.
- the non-woven fabric may be a non-woven fabric composed of short fibers (that is, staples) (short-fiber non-woven fabric) or a non-woven fabric composed of long fibers (that is, filaments) (long-fiber non-woven fabric).
- the staples may generally have a fiber length of several hundred mm or less.
- the core wrap sheets 20a and 20b are laminated including a thermal bond non-woven fabric, an air-through non-woven fabric, a resin bond non-woven fabric, a spunbond non-woven fabric, a melt blow non-woven fabric, an air-laid non-woven fabric, a spunlace non-woven fabric, a point bond non-woven fabric, or two or more kinds of non-woven fabrics selected from these. It can be a body.
- the non-woven fabric used as the core wrap sheets 20a and 20b can be a non-woven fabric formed of synthetic fibers, natural fibers, or a combination thereof.
- synthetic fibers include polyolefins such as polyethylene (PE) and polypropylene (PP), polyesters such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN), polyamides such as nylon, and Examples thereof include fibers containing a synthetic resin selected from rayon.
- Examples of natural fibers include fibers containing cotton, silk, hemp, or pulp (cellulose).
- the fibers forming the non-woven fabric may be polyolefin fibers, polyester fibers or a combination thereof.
- the core wrap sheets 20a and 20b may be tissues.
- the water-absorbing core 50 is sandwiched between, for example, the water-absorbent resin particles 10a or a mixture containing the water-absorbent resin particles 10a and the fibrous material and the core wrap sheets 20a and 20b, and the formed structure is heated as necessary. It can be obtained by the method of pressurizing. If necessary, an adhesive is placed between the core wrap sheets 20a and 20b and the water-absorbent resin particles 10a or a mixture containing the same.
- the water-absorbing core substantially includes a fiber layer as a whole, in addition to the water-absorbing core in which the core wrap sheet 20a, the water-absorbent resin particles 10a, the absorption layer 10 composed of the fiber layer 10b, and the core wrap sheet 20b are arranged in this order. It may be in the form of no sheet.
- FIG. 4 is a cross-sectional view of the water absorption core formed in a sheet shape, showing another example of the water absorption core.
- the 4 includes a core wrap sheet 25a, an adhesive 26a, an absorption layer 10A made of water-absorbent resin particles, a core wrap sheet 25b, an absorption layer 10B made of water-absorbent resin particles, an adhesive 26b, and a core wrap.
- the sheets 25c are arranged in this order.
- the water-absorbent resin particles contained in the absorption layers 10A and 10B may be of the same type or different types.
- the mass and thickness of each of the absorption layers 10A and 10B per unit area may be the same or different.
- the liquid permeable sheet 30 is arranged at the position of the outermost layer on the side where the liquid to be absorbed enters.
- the liquid permeable sheet 30 is arranged on the outside of the core wrap sheet 20b in contact with the core wrap sheet 20b.
- the liquid permeable sheet 40 is arranged at the position of the outermost layer on the side opposite to the liquid permeable sheet 30 in the absorbent article 100.
- the liquid impermeable sheet 40 is arranged on the outside of the core wrap sheet 20a in contact with the core wrap sheet 20a.
- the liquid permeable sheet 30 and the liquid permeable sheet 40 have a main surface wider than the main surface of the water absorbing core 50, and the outer edges of the liquid permeable sheet 30 and the liquid permeable sheet 40 are an absorbing layer.
- the magnitude relationship of the absorbent layer 10, the core wrap sheets 20a and 20b, the auxiliary sheet 60, the liquid permeable sheet 30, and the liquid permeable sheet 40 is appropriately adjusted according to the use of the absorbent article and the like.
- the liquid permeable sheet 30 may be a non-woven fabric.
- the non-woven fabric used as the liquid permeable sheet 30 may have appropriate hydrophilicity from the viewpoint of the liquid absorption performance of the absorbent article. From this point of view, the liquid permeable sheet 30 is a pulp and paper test method No. 1 by the Paper and Pulp Technology Association. A non-woven fabric having a hydrophilicity of 5 to 200 measured according to the measuring method of 68 (2000) may be used. The hydrophilicity of the non-woven fabric may be 10 to 150. Pulp and paper test method No. For details of 68, for example, WO2011 / 086843 can be referred to.
- the non-woven fabric having hydrophilicity may be formed of fibers showing appropriate hydrophilicity such as rayon fiber, or obtained by hydrophilizing a hydrophobic chemical fiber such as polyolefin fiber or polyester fiber. It may be formed of rayon fibers.
- a method for obtaining a non-woven fabric containing hydrophobic chemical fibers that have been hydrophobized for example, a method for obtaining a non-woven fabric by a spunbond method using a mixture of hydrophobic chemical fibers and a hydrophilic agent, hydrophobic chemistry.
- Examples thereof include a method of accommodating a hydrophilic agent when producing a spunbonded nonwoven fabric from fibers, and a method of impregnating a spunbonded nonwoven fabric obtained by using a hydrophobic chemical fiber with a hydrophilic agent.
- the hydrophilizing agent include anionic surfactants such as aliphatic sulfonates and higher alcohol sulfates, cationic surfactants such as quaternary ammonium salts, polyethylene glycol fatty acid esters, polyglycerin fatty acid esters, and sorbitan fatty acids.
- Nonionic surfactants such as esters, silicone-based surfactants such as polyoxyalkylene-modified silicones, and stain-releasing agents made of polyester-based, polyamide-based, acrylic-based, and urethane-based resins are used.
- the amount of texture (mass per unit area) of the non-woven fabric used as the liquid permeable sheet 30 is from the viewpoint of imparting good liquid permeability, flexibility, strength and cushioning property to the absorbent article, and the liquid of the absorbent article. From the viewpoint of increasing the permeation rate, it may be 5 to 200 g / m 2 , 8 to 150 g / m 2 , or 10 to 100 g / m 2 .
- the thickness of the liquid permeable sheet 30 may be 20 to 1400 ⁇ m, 50 to 1200 ⁇ m, or 80 to 1000 ⁇ m.
- the liquid impermeable sheet 40 prevents the liquid absorbed by the absorption layer 10 or the resin layer 61 from leaking to the outside from the liquid impermeable sheet 40 side.
- the liquid impermeable sheet 40 may be a resin sheet or a non-woven fabric.
- the resin sheet may be a sheet made of a synthetic resin such as polyethylene, polypropylene, or polyvinyl chloride.
- the non-woven fabric may be a spunbond / melt blow / spunbond (SMS) non-woven fabric in which a water resistant melt blow non-woven fabric is sandwiched between high-strength spunbond non-woven fabrics.
- SMS spunbond / melt blow / spunbond
- the liquid permeable sheet 40 may be a composite sheet of a resin sheet and a non-woven fabric (for example, a spunbonded non-woven fabric or a spunlaced non-woven fabric).
- the liquid impermeable sheet 40 may have breathability from the viewpoint that stuffiness at the time of wearing is reduced and discomfort given to the wearer can be reduced.
- a sheet of low density polyethylene (LDPE) resin can be used as the liquid impermeable sheet 40 having breathability.
- the basis weight (mass per unit area) of the liquid impermeable sheet 40 is 5 to 100 g / m 2 or 10 to 50 g / m 2. It may be.
- the absorbent article 100 can be manufactured, for example, by a method including arranging the water absorbing core 50 and the auxiliary sheet 60 between the liquid permeable sheet 30 and the liquid impermeable sheet 40.
- a laminate in which the liquid impermeable sheet 40, the auxiliary sheet 60, the water absorption core 50, and the liquid permeable sheet 30 are laminated in this order is pressurized as necessary.
- the absorbent article 100 can also be obtained by arranging the permeable sheets 40 in this order and pressurizing the formed structure while heating if necessary.
- each structural unit may be bonded with an adhesive.
- the first-stage monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, 6.62 g of n-heptane was added as a surfactant to the sucrose stearic acid ester of HLB3. Mitsubishi Chemical Foods Co., Ltd., Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution dissolved by heating is further added, and the inside of the system is sufficiently filled with nitrogen while stirring at a stirring speed of 550 rpm. After the replacement, the flask was immersed in a water bath at 70 ° C. to raise the temperature, and polymerization was carried out for 60 minutes to obtain a first-stage polymerization slurry solution.
- ⁇ Second stage polymerization reaction> Take 128.8 g (1.44 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer in a beaker having an internal volume of 500 mL, and while cooling from the outside, 27 mass% sodium hydroxide. After 159.0 g of the aqueous solution was added dropwise to neutralize 75 mol%, 0.090 g (0.333 mmol) of potassium persulfate was used as the water-soluble radical polymerization initiator, and ethylene glycol diglycidyl ether was used as the internal cross-linking agent. 0116 g (0.067 mmol) was added and dissolved to prepare a second-stage monomer aqueous solution.
- the entire amount of the monomer aqueous solution in the second stage is added to the polymerized slurry liquid in the first stage.
- the flask was again immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization reaction was carried out for 60 minutes to obtain a hydrogel polymer.
- n-heptane and water were heated in an oil bath at 125 ° C. to evaporate and dry to obtain a dried product of polymer particles.
- the polymer particles are passed through a sieve having an opening of 850 ⁇ m, and 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) with respect to the mass of the polymer particles is mixed with the polymer particles.
- amorphous silica Oriental Silicas Corporation, Toxile NP-S
- 233.0 g of water-absorbent resin particles A containing amorphous silica were obtained.
- the medium particle size of the water-absorbent resin particles A was 128 ⁇ m.
- the first-stage monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, 6.62 g of n-heptane was added as a surfactant to the sucrose stearic acid ester of HLB3. Mitsubishi Chemical Foods Co., Ltd., Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution dissolved by heating is further added, and the inside of the system is sufficiently filled with nitrogen while stirring at a stirring speed of 550 rpm. After the replacement, the flask was immersed in a water bath at 70 ° C. to raise the temperature, and polymerization was carried out for 60 minutes to obtain a first-stage polymerization slurry solution.
- ⁇ Second stage polymerization reaction> Take 128.8 g (1.44 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer in a beaker having an internal volume of 500 mL, and while cooling from the outside, 27 mass% sodium hydroxide. After 159.0 g of the aqueous solution was added dropwise to neutralize 75 mol%, 0.129 g (0.476 mmol) of 2,2'-azobis (2-amidinopropane) dihydrochloride as a water-soluble radical polymerization initiator.
- the entire amount of the monomer aqueous solution in the second stage is added to the polymerized slurry liquid in the first stage.
- the inside of the system was replaced with nitrogen for 30 minutes, and then the flask was again immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization reaction was carried out for 60 minutes. As a result, a hydrogel polymer was obtained.
- n-heptane and water were heated in an oil bath at 125 ° C. to evaporate and dry to obtain a dried product of polymer particles.
- the polymer particles are passed through a sieve having an opening of 850 ⁇ m, 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) is mixed with respect to the mass of the polymer particles, and a water-absorbent resin is mixed. 228.5 g of particle C was obtained.
- the medium particle size of the water-absorbent resin particles C was 354 ⁇ m.
- Manufacturing example 4 229.0 g of water-absorbent resin particles D were obtained in the same manner as in Production Example 3 except that 216.7 g of water was extracted from the system by azeotropic distillation.
- the medium particle size of the water-absorbent resin particles D was 348 ⁇ m.
- Production example 5 Water-absorbent resin particles E227.6 g were obtained in the same manner as in Production Example 3 except that 201.4 g of water was extracted from the system by azeotropic distillation.
- the medium particle size of the water-absorbent resin particles E was 356 ⁇ m.
- Production example 6 Inner diameter 11 cm, contents equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirrer (a stirrer blade having two stages of four inclined paddle blades (surface treated with fluororesin) with a blade diameter of 5 cm).
- n-heptane as a hydrocarbon dispersion medium
- sorbitan monolaurate Naonion LP-20R, HLB value: 8.6, manufactured by NOF CORPORATION
- the mixture was obtained by addition.
- the sorbitan monolaurate was dissolved in n-heptane by heating the mixture to 50 ° C. while stirring at a stirring speed of 300 rpm, and then the mixture was cooled to 40 ° C.
- the inside of the system was sufficiently replaced with nitrogen. Then, the flask was immersed in a water bath at 70 ° C. while stirring at a rotation speed of 700 rpm of the stirrer, and then held for 60 minutes to complete the polymerization, thereby obtaining a hydrogel polymer.
- amorphous silica (Oriental Silicas Corporation, oriental silicas corporation, etc.) was added to the polymer solution containing the produced hydrogel polymer, n-heptane and a surfactant as a powdery inorganic flocculant.
- the flask containing the reaction solution was immersed in an oil bath at 125 ° C., and 98.0 g of water was extracted from the system while refluxing n-heptane by azeotropic distillation of n-heptane and water. Then, 4.14 g (ethylene glycol diglycidyl ether: 0.475 mmol) of 2% by mass of an ethylene glycol diglycidyl ether aqueous solution was added as a surface cross-linking agent, and the mixture was maintained at an internal temperature of 83 ⁇ 2 ° C. for 2 hours.
- ethylene glycol diglycidyl ether 0.475 mmol
- water and n-heptane were heated in an oil bath at 125 ° C. to evaporate, and dried until almost no evaporation from the system was distilled off to obtain a dried product of polymer particles.
- the polymer particles were passed through a sieve having an opening of 850 ⁇ m to obtain 90.1 g of water-absorbent resin particles F.
- the medium particle size of the water-absorbent resin particles F was 352 ⁇ m.
- Production example 7 90.6 g of water-absorbent resin particles G were obtained in the same manner as in Production Example 6 except that the powdery inorganic flocculant was not added to the hydrogel polymer.
- the medium particle size of the water-absorbent resin particles G was 156 ⁇ m.
- Production Example 8 104.0 g of water was extracted from the system by azeotropic distillation, and the surface cross-linking agent was changed to 8.28 g of an ethylene glycol diglycidyl ether aqueous solution (ethylene glycol diglycidyl ether: 0.951 mmol). Except for the above, 90.3 g of water-absorbent resin particles H were obtained in the same manner as in Production Example 6. The medium particle size of the water-absorbent resin particles H was 420 ⁇ m.
- Production Example 11 In the preparation of the water-containing gel polymer in the second stage, the temperature inside the separable flask was changed to 28 ° C instead of 31 ° C, and 234.7 g of water was extracted from the system by azeotropic distillation. 230.1 g of water-absorbent resin particles L were obtained in the same manner as in Production Example 3 except that no surfactant was added after the surface cross-linking step. The medium particle size of the water-absorbent resin particles L was 308 ⁇ m.
- Production Example 12 In the preparation of the water-containing gel polymer in the second stage, the temperature in the separable flask was changed to 25 ° C instead of 31 ° C, and in the water-containing gel polymer after the polymerization in the second stage, co-boiling was performed. Similar to Production Example 1, except that 256.5 g of water was extracted from the system by distillation, no surfactant was added after the surface cross-linking step, and amorphous silica was not mixed. 227.2 g of water-absorbent resin particles M were obtained. The medium particle size of the water-absorbent resin particles M was 351 ⁇ m.
- Production example 14 A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
- a maleic anhydride-modified ethylene-propylene copolymer Mitsubishi Chemicals Co., Ltd., High Wax 1105A
- the monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, sucrose stearic acid ester of HLB3 as a surfactant in 6.62 g of n-heptane (Mitsubishi Chemical Foods Co., Ltd.) , Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution is further added, and the inside of the system is sufficiently replaced with nitrogen while stirring at a stirring speed of 400 rpm, and then the flask.
- the flask was immersed in an oil bath set at 125 ° C., and 116 g of water was extracted from the system while refluxing n-heptane by azeotropic distillation of n-heptane and water. Then, 1.84 g (0.211 mmol) of a 2% by mass ethylene glycol diglycidyl ether aqueous solution was added to the flask as a surface cross-linking agent, and the flask was kept at 83 ° C. for 2 hours.
- n-heptane and water were evaporated at 125 ° C. and dried to obtain a dried product of polymer particles.
- the polymer particles are passed through a sieve having an opening of 850 ⁇ m, and 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) with respect to the mass of the polymer particles is mixed with the polymer particles.
- 90.9 g of water-absorbent resin particles P containing amorphous silica were obtained.
- the medium particle size of the water-absorbent resin particles P was 422 ⁇ m.
- the medium particle size of the particles was measured by the following procedure. That is, from the top, the JIS standard sieve has a mesh size of 600 ⁇ m, a mesh size of 500 ⁇ m, a mesh size of 425 ⁇ m, a mesh size of 300 ⁇ m, a mesh size of 250 ⁇ m, a mesh size of 180 ⁇ m, and a mesh size of 150 ⁇ m. , And the saucer in that order. 50 g of particles were placed in the best combined sieve and classified according to JIS Z 8815 (1994) using a low-tap shaker (manufactured by Iida Seisakusho Co., Ltd.).
- the mass of the particles remaining on each sieve was calculated as a mass percentage with respect to the total amount, and the particle size distribution was obtained.
- the relationship between the mesh size of the sieve and the integrated value of the mass percentage of the particles remaining on the sieve was plotted on a logarithmic probability paper by integrating the particle size distribution on the sieve in order from the largest particle size. By connecting the plots on the probability paper with a straight line, the particle size corresponding to the cumulative mass percentage of 50% by mass was obtained as the medium particle size.
- Air-laid non-woven fabric-2 with hot melt coating machine (Henkel Co., Ltd., pump: Marshal150, table: XA-DT, tank set temperature: 150 ° C, hose set temperature: 165 ° C, gun head set temperature: 170 ° C)
- 0.2 g of hot melt adhesive (Henkel Japan Ltd., ME-765E) was applied in 12 linear lines at 10 mm intervals.
- the adhesive application pattern was a spiral stripe.
- the surface of the air-laid non-woven fabric-2 to which the hot melt was attached was aligned with the surface on which the water-absorbent resin particles of the air-through non-woven fabric were sprayed, and sandwiched between release papers and turned upside down. Then, the release paper and the air-laid non-woven fabric-1 were removed.
- the water absorption core A has the same configuration as the water absorption core shown in FIG.
- Production example 16 Water-absorbent resin particles (Aquakeep SA60S manufactured by Sumitomo Seika Chemical Co., Ltd., water absorption of physiological saline 60 g / g, medium particle diameter 342 ⁇ m) using an air flow type mixer (Padformer manufactured by Otec Co., Ltd.) A sheet-shaped absorbent layer having a size of 40 cm ⁇ 10 cm was prepared by uniformly mixing 12.0 g and 3.0 g of pulverized pulp by air papermaking.
- water absorption is performed by applying a load of 196 kPa to the entire surface for 30 seconds with the upper and lower sides of the absorbent layer sandwiched between two sheets of tissue having the same size as the sheet-shaped absorbent layer and having a basis weight of 16 g / m 2.
- the core was made. This was designated as the water absorption core B.
- the produced water-absorbing core B has an absorbing layer made of water-absorbing resin particles and crushed pulp arranged between two sheets of tissue.
- Example 1 (Preparation of auxiliary sheet) Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 14 cm ⁇ 42 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (3M Spray Glue 77 manufactured by 3M Japan Ltd.) to the inner surface of the roll of the lower sheet base material, promptly airflow type mixing device (manufactured by Otec Co., Ltd., pad former) ) was used to uniformly spray 1.5 g of the water-absorbent resin particles A prepared in Production Example 1 over a range of 10 cm ⁇ 40 cm in the center of the lower sheet base material.
- adhesive 3M Spray Glue 77 manufactured by 3M Japan Ltd.
- an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to the upper sheet base material.
- the surface coated with the adhesive of the upper sheet base material is overlapped with the surface on which the water-absorbent resin of the lower sheet base material is sprayed, with both ends aligned, and the entire surface is adhered to the area where the water-absorbent resin is sprayed. (10 cm ⁇ 40 cm) was cut out to obtain an auxiliary sheet.
- Example 2 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles B produced in Production Example 2.
- Example 3 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles C produced in Production Example 3.
- Example 4 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles D produced in Production Example 4.
- Example 5 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles E produced in Production Example 5.
- Example 6 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6.
- Example 7 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles G produced in Production Example 7.
- Example 8 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles H produced in Production Example 8.
- Example 9 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles J produced in Production Example 9.
- Example 10 The upper sheet base material and the lower sheet base material of the auxiliary sheet were changed to spunbonded non-woven fabric (manufactured by Toray Polytech (Nantong) Co., Ltd., trade name: LIVESEN) having a basis weight of 17 g / m 2.
- An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the sheet were changed to the water-absorbent resin particles F produced in Production Example 6.
- Example 11 The upper sheet base material and the lower sheet base material of the auxiliary sheet were changed to air-through non-woven fabric manufactured by Rengo Nonwoven Products Co., Ltd. with a grain size of 21 g / m 2, and water-absorbent resin particles for the auxiliary sheet were produced.
- An absorbent article was obtained in the same manner as in Example 1 except that the particles were changed to the water-absorbent resin particles F produced in 1.
- Example 12 The upper sheet base material of the auxiliary sheet was changed to an air-through non-woven fabric manufactured by Hualong (Nanjining) with a grain size of 45 g / m 2, and the water-absorbent resin particles for the auxiliary sheet were prepared in Production Example 6. An absorbent article was obtained in the same manner as in Example 1 except that it was changed to F.
- Example 13 (Preparation of auxiliary sheet) By using an air flow type mixer (Padformer manufactured by Otec Co., Ltd.) to uniformly mix 1.5 g of the water-absorbent resin particles F and 1.5 g of crushed pulp of Production Example 6 by air papermaking, the size is 40 cm ⁇ 10 cm. A sheet-shaped resin layer having a size was prepared. Next, a load of 196 kPa is applied to the entire surface for 30 seconds while the resin layer is sandwiched between two sheets of tissue having the same size as the sheet-shaped resin layer and having a grain size of 16 g / m 2, and pressed. An auxiliary sheet was obtained in which a resin layer composed of water-absorbent resin particles and crushed pulp was arranged between two sheets of tissue.
- an air flow type mixer Padformer manufactured by Otec Co., Ltd.
- Example 14 The same as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6 and the amount of the water-absorbent resin particles used was changed to 1.0 g. An absorbent article was obtained.
- Example 15 An auxiliary sheet was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6.
- the water-absorbing core B produced in Production Example 16 was placed on the obtained auxiliary sheet to obtain an absorbent article.
- Example 16 The same as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6 and the amount of the water-absorbent resin particles used was changed to 0.4 g. An absorbent article was obtained.
- Comparative Example 1 Only the water-absorbing core A produced in Production Example 15 without using the auxiliary sheet was used as the absorbent article for the test.
- the water-absorbing core was prepared in the same manner as in Production Example 15 except that the amount of the water-absorbent resin particles sprayed between the air-laid non-woven fabric-2 and the air-through non-woven fabric of Production Example 15 was changed from 6.0 g to 5.0 g. Obtained. Only the above-mentioned water-absorbing core obtained without using the auxiliary sheet was used as an absorbent article for testing.
- Comparative Example 3 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles were not used.
- Comparative Example 4 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles K produced in Production Example 10.
- Comparative Example 5 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles L produced in Production Example 11.
- Comparative Example 6 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles M produced in Production Example 12.
- Comparative Example 7 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles N produced in Production Example 13.
- Comparative Example 8 An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles P produced in Production Example 14.
- dry powder passing liquid absorption rate dry powder passing liquid absorbing amount (g) / 0.2 g artificial urine saturated liquid absorbing amount (g) of the water-absorbent resin.
- dry powder passing liquid absorption amount and the artificial urine saturated liquid absorption amount of 0.2 g were measured and calculated by the methods shown below.
- FIG. 5 is a schematic view showing a method for measuring the liquid absorption rate of dry powder.
- 61a was uniformly sprayed, and the total mass Wb of the container and the water-absorbent resin particles 61a sprayed in the container was measured.
- a plastic beaker with an opening diameter of 60 mm and a height of 70 mm was used as the receiver 53, and the cylindrical container 52 was placed on the receiver 53.
- the dropping funnel 54 was installed so that the distance H between the tip 54a and the upper surface of the mesh 51 was 13 mm and the tip 54a was located above the center of the bottom surface of the cylindrical container 52.
- Artificial urine 45 (20 mL) adjusted to a liquid temperature of 25 ° C. was injected at a constant rate of 8 mL / sec, and the stopwatch was started at the same time.
- the artificial urine diffuses over the entire bottom surface of the cylindrical container 52, passes through the mesh 51 and falls into the receiver 53, but a part of the artificial urine is absorbed by the water-absorbent resin particles 61a.
- the water-absorbent resin particles 61a absorb the artificial urine 45 to form a swollen gel.
- the total mass Wa of the cylindrical container 52 and the swollen gel in the cylindrical container 52 was measured.
- the amount of dry powder flowing through the liquid (g) was determined by Wa-Wb.
- the mass Wd (g) of the sieve containing the swelling gel was measured, and the artificial urine saturated liquid absorption amount was determined by the following formula.
- -Artificial urine saturated liquid absorption (g / g) (Wd-Wc) /2.0
- -0.2 g of artificial urine saturated liquid absorption (g) 0.2 x artificial urine saturated liquid absorption (g / g)
- auxiliary sheet thickness evaluation The thickness of the auxiliary sheet was measured using a precision thickness measuring instrument (manufactured by Ozaki Seisakusho, dial thickness gauge JB, stylus: aluminum ⁇ 50 mm). The measurement was performed at a position where the stylus was in contact with the central portion of the auxiliary sheet, and the average of the values measured three times was taken as the thickness (mm) of the auxiliary sheet.
- FIG. 6 is a schematic view showing an apparatus for evaluating liquid leakage of an absorbent article.
- the liquid leakage property at the initial stage of liquid absorption of the absorbent article 100 for testing was evaluated by the following procedures (i), (ii), (iii) and (iv). ..
- the results are shown in Table 1.
- the resin in the table represents water-absorbent resin particles, and gsm represents g / m 2 .
- (I) is a mechanical fastener (3M mechanical fastener hook), vertical 45cm, was cut to the size of the acrylic resin plate 1 having a rectangular main surface of the lateral 62cm, was adhered to the entire main surface S 1 of the acrylic resin plate 1.
- On the main surface S 1 of the acrylic resin plate 1 is extremely fine irregularities are caused by mechanical fasteners, no retention and absorption of liquids on the main surface S 1 of the acrylic resin plate 1.
- the long side of the acrylic resin plate 1 was parallel to the horizontal plane, and the main surface of the acrylic resin plate 1 and the horizontal plane S 0 were fixed so as to form 45 ⁇ 2 degrees.
- a fixed main surface S 1 of the acrylic resin plate 1, the absorbent article 100 for testing, in a direction that long sides are perpendicular to the long side of the acrylic resin plate 1, an absorbent article for testing 100 The lower end of the acrylic resin plate 1 was attached so as to be at the same position as the lower end of the acrylic resin plate 1.
- the test absorbent article 100 composed of the water absorption core and the auxiliary sheet was attached on the acrylic resin plate 1 so that the water absorption core was on the front side.
- the upper end of the absorbent article 100 for testing was fixed to the acrylic resin plate 1 with an adhesive tape to prevent it from falling.
- the loading point is 8 cm above the center of the absorption core in the absorbent article 100 for testing, and from a position 1 cm vertically above the loading point, the dropping funnel 42 (300 mL of dropping funnel manufactured by Cosmos Bead Co., Ltd., tip) An inner diameter of 8 mm ⁇ 6 mm) was used to inject a predetermined amount of artificial urine 45 adjusted to a liquid temperature of 25 ° C. at a rate of 8 mL / sec.
- the injection amount of artificial urine 45 when using the water-absorbing core A having an absorption layer made of water-absorbent resin particles is 80 mL, and when using the water-absorbing core B having an absorption layer made of water-absorbent resin particles and crushed pulp.
- the injection amount of artificial urine 45 was 120 mL (Examples or comparative examples marked with * in Table 1).
- (Iv) The artificial urine leaked from the absorbent article 100 for testing was collected in a metal tray 44 previously placed below the absorbent article 100 and placed on the balance. The collected artificial urine was weighed, and the ratio (%) of the amount of leaked artificial urine (g) to the input amount (g) of artificial urine was calculated.
- Table 1 shows the evaluation results. It has been shown that an absorbent article having an auxiliary sheet prepared by using water-absorbent resin particles having a dry powder passing liquid absorption rate of a specific numerical value improves liquid leakage in the initial stage of liquid absorption.
- 10, 10A, 10B Absorbent layer, 10a ... Water-absorbent resin particles, 10b ... Fiber layer, 20a, 20b ... Core wrap sheet, 21 ... Adhesive, 25a, 25b, 25c ... Core wrap sheet, 26a, 26b ... Adhesive , 30 ... Liquid permeable sheet, 40 ... Liquid permeable sheet, 50 ... Water absorption core, 51 ... Mesh (mesh-like bottom), 52 ... Cylindrical container, 60 ... Auxiliary sheet, 61 ... Resin layer, 61a ... Water absorption Sex resin particles, 61b ... fiber layer, 62a, 62b ... sheet base material, 63a, 63b ... adhesive, 100 ... absorbent article.
- 10a Water-absorbent resin particles, 10b ... Fiber layer, 20a, 20b ... Core wrap sheet, 21 ... Adhesive, 25a, 25b, 25c ... Core wrap sheet, 26a, 26
Abstract
Description
(1)メッシュ状の底部を備える内径60mmの円筒状容器内の底面全体にわたり、0.2gの吸水性樹脂粒子を均一に散布し、容器及び該容器内に散布された吸水性樹脂粒子の合計質量Wb(g)を測定する。
(2)吸水性樹脂粒子が散布された容器内に液温25℃の人工尿20mLを8mL/秒の一定速度で注入し、人工尿の少なくとも一部を吸水性樹脂粒子に吸液させて容器内で膨潤ゲルを形成させる。
(3)注入開始から30秒後に、容器及び該容器内の膨潤ゲルの合計質量Wa(g)を測定する。
(4)Wa(g)-Wb(g)により乾粉通液吸液量(g)を求める。
(5)0.2gの吸水性樹脂粒子の人工尿飽和吸液量(g)に対する乾粉通液吸液量(g)の比として、乾粉通液吸液率(g/g)を得る。 One aspect of the present invention includes a water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet and a liquid permeable sheet, and includes a liquid impermeable sheet, an auxiliary sheet, a water absorbing core and a liquid permeable sheet. With respect to absorbent articles in which the sheets are arranged in this order. In the absorbent article, the auxiliary sheet includes a resin layer containing water-absorbent resin particles, and the following steps (1), (2), (3), (4) and (5) are included in this order. The measured dry powder passing liquid absorption rate of the water-absorbent resin particles is 0.25 or more and 1.0 or less.
(1) 0.2 g of water-absorbent resin particles are uniformly sprayed over the entire bottom surface of a cylindrical container having an inner diameter of 60 mm having a mesh-like bottom, and the total amount of the container and the water-absorbent resin particles sprayed in the container. The mass Wb (g) is measured.
(2) 20 mL of artificial urine having a liquid temperature of 25 ° C. is injected into the container on which the water-absorbent resin particles are sprayed at a constant rate of 8 mL / sec, and at least a part of the artificial urine is absorbed by the water-absorbent resin particles to make the container. A swelling gel is formed within.
(3) 30 seconds after the start of injection, the total mass Wa (g) of the container and the swollen gel in the container is measured.
(4) The dry powder passing liquid absorption amount (g) is determined from Wa (g) -Wb (g).
(5) The dry powder passage liquid absorption rate (g / g) is obtained as the ratio of the dry powder passage liquid absorption amount (g) to the artificial urine saturated liquid absorption amount (g) of 0.2 g of the water-absorbent resin particles.
(1)メッシュ状の底部を備える内径60mmの円筒状容器内の底面全体にわたり、0.2gの吸水性樹脂粒子を均一に散布し、容器及び該容器内に散布された吸水性樹脂粒子の合計質量Wb(g)を測定する。
(2)吸水性樹脂粒子が散布された容器内に液温25℃の人工尿20mLを8mL/秒の一定速度で注入し、人工尿の少なくとも一部を吸水性樹脂粒子に吸液させて容器内で膨潤ゲルを形成させる。
(3)注入開始から30秒後に、容器及び該容器内の膨潤ゲルの合計質量Wa(g)を測定する。
(4)Wa(g)-Wb(g)により乾粉通液吸液量(g)を求める。
(5)0.2gの吸水性樹脂粒子の人工尿飽和吸液量(g)に対する乾粉通液吸液量(g)の比として、乾粉通液吸液率(g/g)を得る。 The auxiliary sheet includes a resin layer containing water-absorbent resin particles, and is measured by a method including the following steps (1), (2), (3), (4) and (5) in this order. The dry powder water absorption rate of the resin particles is 0.25 or more and 1.0 or less.
(1) 0.2 g of water-absorbent resin particles are uniformly sprayed over the entire bottom surface of a cylindrical container having an inner diameter of 60 mm having a mesh-like bottom, and the total amount of the container and the water-absorbent resin particles sprayed in the container. The mass Wb (g) is measured.
(2) 20 mL of artificial urine having a liquid temperature of 25 ° C. is injected into the container on which the water-absorbent resin particles are sprayed at a constant rate of 8 mL / sec, and at least a part of the artificial urine is absorbed by the water-absorbent resin particles to make the container. A swelling gel is formed within.
(3) 30 seconds after the start of injection, the total mass Wa (g) of the container and the swollen gel in the container is measured.
(4) The dry powder passing liquid absorption amount (g) is determined from Wa (g) -Wb (g).
(5) The dry powder passage liquid absorption rate (g / g) is obtained as the ratio of the dry powder passage liquid absorption amount (g) to the artificial urine saturated liquid absorption amount (g) of 0.2 g of the water-absorbent resin particles.
(a)500mL容のビーカー内に500gの人工尿を投入する。
(b)人工尿が投入されたビーカー内に、人工尿をマグネチックスターラーバー(8mmφ×30mm、リング無し)を用いて600rpmで攪拌させながら、2.0gの吸水性樹脂粒子を投入する。
(c)吸水性樹脂粒子の投入後60分間人工尿及び吸水性樹脂粒子を600rpmで撹拌して膨潤ゲルを形成させる。
(d)ビーカー内の内容物を目開き75μm標準篩でろ過し、1分間静置して余剰の水分を取り除く。
(e)膨潤ゲル及び篩の合計質量Wcを測定し、予め測定した篩の質量Wdから、次の式により0.2gの人工尿飽和吸液量(g)を求める。
0.2gの人工尿飽和吸液量(g)=0.2×(Wc-Wd)/2.0 The artificial urine saturated liquid absorption amount of 0.2 g of the water-absorbent resin particles is calculated by a method including the following steps (a), (b), (c), (d) and (e) in this order.
(A) Put 500 g of artificial urine into a 500 mL beaker.
(B) 2.0 g of water-absorbent resin particles are charged into the beaker into which the artificial urine is charged while stirring the artificial urine at 600 rpm using a magnetic stirrer bar (8 mmφ × 30 mm, without ring).
(C) The artificial urine and the water-absorbent resin particles are stirred at 600 rpm for 60 minutes after the water-absorbent resin particles are added to form a swollen gel.
(D) The contents in the beaker are filtered through a 75 μm standard sieve with an opening, and allowed to stand for 1 minute to remove excess water.
(E) The total mass Wc of the swollen gel and the sieve is measured, and 0.2 g of the artificial urine saturated liquid absorption amount (g) is obtained from the previously measured mass Wd of the sieve by the following formula.
0.2 g artificial urine saturated liquid absorption amount (g) = 0.2 × (Wc-Wd) /2.0
エチレン性不飽和単量体は水溶性であってもよい。水溶性エチレン性不飽和単量体の例としては、(メタ)アクリル酸及びその塩、2-(メタ)アクリルアミド-2-メチルプロパンスルホン酸及びその塩、(メタ)アクリルアミド、N,N-ジメチル(メタ)アクリルアミド、2-ヒドロキシエチル(メタ)アクリレート、N-メチロール(メタ)アクリルアミド、ポリエチレングリコールモノ(メタ)アクリレート、N,N-ジエチルアミノエチル(メタ)アクリレート、N,N-ジエチルアミノプロピル(メタ)アクリレート、ジエチルアミノプロピル(メタ)アクリルアミド等が挙げられる。エチレン性不飽和単量体がアミノ基を有する場合、当該アミノ基は4級化されていてもよい。エチレン性不飽和単量体は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。上述の単量体のカルボキシル基、アミノ基等の官能基は、後述する表面架橋工程において架橋が可能な官能基として機能し得る。 <Water-absorbent resin particles>
The ethylenically unsaturated monomer may be water-soluble. Examples of water-soluble ethylenically unsaturated monomers include (meth) acrylic acid and its salts, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts, (meth) acrylamide, N, N-dimethyl. (Meta) acrylamide, 2-hydroxyethyl (meth) acrylate, N-methylol (meth) acrylamide, polyethylene glycol mono (meth) acrylate, N, N-diethylaminoethyl (meth) acrylate, N, N-diethylaminopropyl (meth) Examples thereof include acrylate and diethylaminopropyl (meth) acrylamide. When the ethylenically unsaturated monomer has an amino group, the amino group may be quaternized. The ethylenically unsaturated monomer may be used alone or in combination of two or more. Functional groups such as the carboxyl group and amino group of the above-mentioned monomers can function as functional groups capable of cross-linking in the surface cross-linking step described later.
含水率=[Ww/(Ww+Ws)]×100
Ww:全重合工程の重合前の単量体水溶液に含まれる水分量から、乾燥工程等により系外部に排出された水分量を差し引いた量に、凝集剤、表面架橋剤等を混合する際に必要に応じて用いられる水分量を加えることで算出される含水ゲル状重合体の水分量。 In the production of the water-absorbent resin particles, even if the surface portion of the hydrogel polymer is crosslinked (surface crosslink) using a cross-linking agent in any of the drying step (moisture removing step) and subsequent steps. Good. By performing surface cross-linking, it is easy to control the water absorption characteristics of the water-absorbent resin particles. The water content of the surface-crosslinked hydrogel polymer may be 5 to 50% by mass, 10 to 40% by mass, or 15 to 35% by mass. The water content (mass%) of the water-containing gel polymer is calculated by the following formula.
Moisture content = [Ww / (Ww + Ws)] x 100
Ww: When the flocculant, surface cross-linking agent, etc. are mixed in the amount obtained by subtracting the amount of water discharged to the outside of the system by the drying step or the like from the amount of water contained in the monomer aqueous solution before polymerization in the total polymerization step. The amount of water in the hydrogel polymer calculated by adding the amount of water used as needed.
図1は、補助シートの一例を示す断面図である。図1に示す補助シート60は、樹脂層61と、2枚のシート基材62a,62bとを有する。シート基材62a,62bは、樹脂層61の両側に配置されている。言い換えると、樹脂層61は、シート基材62a,62bの内側に配置されている。樹脂層61は、2枚のシート基材62a,62bの間に挟まれることにより、保形されている。シート基材62a,62bは、2枚のシートであってもよいし、折り返された1枚のシート、又は1枚の袋体であってもよい。 <Auxiliary sheet>
FIG. 1 is a cross-sectional view showing an example of an auxiliary sheet. The
図2は、吸収性物品の一例を示す断面図である。図2に示す吸収性物品100は、吸水コア50と、補助シート60と、液体透過性シート30と、液体不透過性シート40とを備える。言い換えると、吸水コア50と補助シート60が、液体透過性シート30と液体不透過性シート40との間に挟まれている。 <Absorbable article>
FIG. 2 is a cross-sectional view showing an example of an absorbent article. The
製造例1
<第1段目の重合反応>
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 [Preparation of water-absorbent resin particles]
Manufacturing example 1
<First stage polymerization reaction>
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
内容積500mLのビーカーに水溶性エチレン性不飽和単量体として80.5質量%のアクリル酸水溶液128.8g(1.44モル)をとり、外部より冷却しつつ、27質量%の水酸化ナトリウム水溶液159.0gを滴下して75モル%の中和を行った後、水溶性ラジカル重合開始剤として過硫酸カリウム0.090g(0.333ミリモル)、内部架橋剤としてエチレングリコールジグリシジルエーテル0.0116g(0.067ミリモル)を加えて溶解し、第2段目の単量体水溶液を調製した。 <Second stage polymerization reaction>
Take 128.8 g (1.44 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer in a beaker having an internal volume of 500 mL, and while cooling from the outside, 27 mass% sodium hydroxide. After 159.0 g of the aqueous solution was added dropwise to neutralize 75 mol%, 0.090 g (0.333 mmol) of potassium persulfate was used as the water-soluble radical polymerization initiator, and ethylene glycol diglycidyl ether was used as the internal cross-linking agent. 0116 g (0.067 mmol) was added and dissolved to prepare a second-stage monomer aqueous solution.
第2段目の含水ゲル状重合体の作製において、セパラブルフラスコ内の温度を31℃に代えて25℃に変更したこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により256.8gの水を系外へ抜き出したこと、重合体粒子と混合する非晶質シリカの量を重合体粒子質量に対して0.5質量%に変更したこと以外は、製造例1と同様にして、吸水性樹脂粒子Bを230.2g得た。吸水性樹脂粒子Bの中位粒子径は358μmであった。 Manufacturing example 2
In the preparation of the hydrogel polymer in the second stage, the temperature in the separable flask was changed to 25 ° C instead of 31 ° C, and in the hydrogel polymer after the polymerization in the second stage, co-boiling was performed. Production Example 1 except that 256.8 g of water was extracted from the system by distillation and the amount of amorphous silica mixed with the polymer particles was changed to 0.5% by mass with respect to the mass of the polymer particles. In the same manner as above, 230.2 g of water-absorbent resin particles B were obtained. The medium particle size of the water-absorbent resin particles B was 358 μm.
<第1段目の重合反応>
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 Manufacturing example 3
<First stage polymerization reaction>
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
内容積500mLのビーカーに水溶性エチレン性不飽和単量体として80.5質量%のアクリル酸水溶液128.8g(1.44モル)をとり、外部より冷却しつつ、27質量%の水酸化ナトリウム水溶液159.0gを滴下して75モル%の中和を行った後、水溶性ラジカル重合開始剤として2,2’-アゾビス(2-アミジノプロパン)2塩酸塩0.129g(0.476ミリモル)、および過硫酸カリウム0.026g(0.096ミリモル)、内部架橋剤としてエチレングリコールジグリシジルエーテル0.0116g(0.067ミリモル)を加えて溶解し、第2段目の単量体水溶液を調製した。 <Second stage polymerization reaction>
Take 128.8 g (1.44 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer in a beaker having an internal volume of 500 mL, and while cooling from the outside, 27 mass% sodium hydroxide. After 159.0 g of the aqueous solution was added dropwise to neutralize 75 mol%, 0.129 g (0.476 mmol) of 2,2'-azobis (2-amidinopropane) dihydrochloride as a water-soluble radical polymerization initiator. , 0.026 g (0.096 mmol) of potassium persulfate, and 0.0116 g (0.067 mmol) of ethylene glycol diglycidyl ether as an internal cross-linking agent are added and dissolved to prepare a second-stage monomer aqueous solution. did.
共沸蒸留により216.7gの水を系外へ抜き出したこと以外は、製造例3と同様にして、吸水性樹脂粒子Dを229.0g得た。吸水性樹脂粒子Dの中位粒子径は348μmであった。 Manufacturing example 4
229.0 g of water-absorbent resin particles D were obtained in the same manner as in Production Example 3 except that 216.7 g of water was extracted from the system by azeotropic distillation. The medium particle size of the water-absorbent resin particles D was 348 μm.
共沸蒸留により201.4gの水を系外へ抜き出したこと以外は、製造例3と同様にして、吸水性樹脂粒子E227.6gを得た。吸水性樹脂粒子Eの中位粒子径は356μmであった。 Production example 5
Water-absorbent resin particles E227.6 g were obtained in the same manner as in Production Example 3 except that 201.4 g of water was extracted from the system by azeotropic distillation. The medium particle size of the water-absorbent resin particles E was 356 μm.
還流冷却器、滴下ロート、窒素ガス導入管、及び、撹拌機(翼径5cmの4枚傾斜パドル翼(フッ素樹脂にて表面処理したもの)を2段有する撹拌翼)を備えた内径11cm、内容積2Lの、4箇所の側壁バッフル付き丸底円筒型セパラブルフラスコ(バッフル長さ:10cmバッフル幅:7mm)を準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン451.4gを添加し、界面活性剤としてソルビタンモノラウレート(ノニオンLP-20R、HLB値:8.6、日油株式会社製)1.288gを添加することにより混合物を得た。この混合物を撹拌機の回転数300rpmで撹拌しつつ50℃まで昇温することによりソルビタンモノラウレートをn-ヘプタンに溶解させた後、混合物を40℃まで冷却した。 Production example 6
Inner diameter 11 cm, contents equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirrer (a stirrer blade having two stages of four inclined paddle blades (surface treated with fluororesin) with a blade diameter of 5 cm). A round-bottomed cylindrical separable flask with a stack of 2 L and four side wall baffles (baffle length: 10 cm, baffle width: 7 mm) was prepared. To this flask, 451.4 g of n-heptane as a hydrocarbon dispersion medium was added, and 1.288 g of sorbitan monolaurate (Nonion LP-20R, HLB value: 8.6, manufactured by NOF CORPORATION) was added as a surfactant. The mixture was obtained by addition. The sorbitan monolaurate was dissolved in n-heptane by heating the mixture to 50 ° C. while stirring at a stirring speed of 300 rpm, and then the mixture was cooled to 40 ° C.
含水ゲル状重合体に粉末状無機凝集剤を添加しなかったこと以外は製造例6と同様にして、吸水性樹脂粒子Gを90.6g得た。吸水性樹脂粒子Gの中位粒子径は156μmであった。 Production example 7
90.6 g of water-absorbent resin particles G were obtained in the same manner as in Production Example 6 except that the powdery inorganic flocculant was not added to the hydrogel polymer. The medium particle size of the water-absorbent resin particles G was 156 μm.
共沸蒸留により104.0gの水を系外へ抜き出したこと、表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液8.28g(エチレングリコールジグリシジルエーテル:0.951ミリモル)に変更したこと以外は製造例6と同様にして、吸水性樹脂粒子Hを90.3g得た。吸水性樹脂粒子Hの中位粒子径は420μmであった。 Production Example 8
104.0 g of water was extracted from the system by azeotropic distillation, and the surface cross-linking agent was changed to 8.28 g of an ethylene glycol diglycidyl ether aqueous solution (ethylene glycol diglycidyl ether: 0.951 mmol). Except for the above, 90.3 g of water-absorbent resin particles H were obtained in the same manner as in Production Example 6. The medium particle size of the water-absorbent resin particles H was 420 μm.
第2段目の含水ゲル状重合体の作製において、セパラブルフラスコ内の温度を31℃に代えて25℃に変更したこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により256.5gの水を系外へ抜き出したこと、重合体粒子と混合する非晶質シリカの量を重合体粒子の質量に対して0.25質量%に変更したこと以外は、製造例1と同様にして、吸水性樹脂粒子Jを228.2g得た。吸水性樹脂粒子Jの中位粒子径は360μmであった。 Manufacturing example 9
In the preparation of the hydrogel polymer in the second stage, the temperature in the separable flask was changed to 25 ° C instead of 31 ° C, and in the hydrogel polymer after the polymerization in the second stage, co-boiling was performed. Production example except that 256.5 g of water was extracted from the system by distillation and the amount of amorphous silica mixed with the polymer particles was changed to 0.25% by mass with respect to the mass of the polymer particles. In the same manner as in 1, 228.2 g of water-absorbent resin particles J was obtained. The medium particle size of the water-absorbent resin particles J was 360 μm.
第1段目の撹拌速度を550rpmから500rpmに変更し、第2段目の含水ゲル状重合体の作製において、セパラブルフラスコ内の温度を31℃に代えて25℃に変更したこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により257.2gの水を系外へ抜き出したこと、表面架橋工程後に界面活性剤を添加しなかったこと以外は、製造例1と同様にして、吸水性樹脂粒子Kを231.2g得た。吸水性樹脂粒子Kの中位粒子径は359μmであった。 Production Example 10
The stirring speed of the first stage was changed from 550 rpm to 500 rpm, and in the preparation of the hydrogel polymer of the second stage, the temperature inside the separable flask was changed to 25 ° C instead of 31 ° C. In the hydrogel polymer after the stage polymerization, 257.2 g of water was extracted from the system by co-boiling distillation, and no surfactant was added after the surface cross-linking step. Similarly, 231.2 g of water-absorbent resin particles K were obtained. The medium particle size of the water-absorbent resin particles K was 359 μm.
第2段目の含水ゲル状重合体の作製において、セパラブルフラスコ内の温度を31℃に代えて28℃に変更したこと、共沸蒸留により234.7gの水を系外へ抜き出したこと、表面架橋工程後に界面活性剤を添加しなかったこと以外は、製造例3と同様にして、吸水性樹脂粒子Lを230.1g得た。吸水性樹脂粒子Lの中位粒子径は308μmであった。 Production Example 11
In the preparation of the water-containing gel polymer in the second stage, the temperature inside the separable flask was changed to 28 ° C instead of 31 ° C, and 234.7 g of water was extracted from the system by azeotropic distillation. 230.1 g of water-absorbent resin particles L were obtained in the same manner as in Production Example 3 except that no surfactant was added after the surface cross-linking step. The medium particle size of the water-absorbent resin particles L was 308 μm.
第2段目の含水ゲル状重合体の作製において、セパラブルフラスコ内の温度を31℃に代えて25℃に変更したこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により256.5gの水を系外へ抜き出したこと、表面架橋工程後に界面活性剤を添加しなかったこと、非晶質シリカを混合しなかったこと以外は、製造例1と同様にして、吸水性樹脂粒子Mを227.2g得た。吸水性樹脂粒子Mの中位粒子径は351μmであった。 Production Example 12
In the preparation of the water-containing gel polymer in the second stage, the temperature in the separable flask was changed to 25 ° C instead of 31 ° C, and in the water-containing gel polymer after the polymerization in the second stage, co-boiling was performed. Similar to Production Example 1, except that 256.5 g of water was extracted from the system by distillation, no surfactant was added after the surface cross-linking step, and amorphous silica was not mixed. 227.2 g of water-absorbent resin particles M were obtained. The medium particle size of the water-absorbent resin particles M was 351 μm.
第2段目の含水ゲル状重合体の作製において、セパラブルフラスコ内の温度を31℃に代えて25℃に変更したこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により256.5gの水を系外へ抜き出したこと、表面架橋工程後に界面活性剤を添加しなかったこと、重合体粒子の質量に対して0.5質量%の非晶質シリカ(東ソー・シリカ株式会社製、Nipsil SS-30P)を重合体粒子と混合したこと以外は、製造例1と同様にして、吸水性樹脂粒子Nを229.2g得た。吸水性樹脂粒子Nの中位粒子径は359μmであった。 Production Example 13
In the preparation of the hydrogel polymer in the second stage, the temperature in the separable flask was changed to 25 ° C instead of 31 ° C, and in the hydrogel polymer after the polymerization in the second stage, co-boiling 256.5 g of water was extracted from the system by distillation, no surfactant was added after the surface cross-linking step, and 0.5% by mass of amorphous silica with respect to the mass of the polymer particles (Tosoh. 229.2 g of water-absorbent resin particles N were obtained in the same manner as in Production Example 1 except that Nipsil SS-30P manufactured by Silica Co., Ltd. was mixed with the polymer particles. The medium particle size of the water-absorbent resin particles N was 359 μm.
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 Production example 14
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
粒子の中位粒子径は下記手順により測定した。すなわち、JIS標準篩を上から、目開き600μmの篩、目開き500μmの篩、目開き425μmの篩、目開き300μmの篩、目開き250μmの篩、目開き180μmの篩、目開き150μmの篩、及び、受け皿の順に組み合わせた。組み合わせた最上の篩に、粒子50gを入れ、ロータップ式振とう器(株式会社飯田製作所製)を用いてJIS Z 8815(1994)に準じて分級した。分級後、各篩上に残った粒子の質量を全量に対する質量百分率として算出し粒度分布を求めた。この粒度分布に関して粒子径の大きい方から順に篩上を積算することにより、篩の目開きと篩上に残った粒子の質量百分率の積算値との関係を対数確率紙にプロットした。確率紙上のプロットを直線で結ぶことにより、積算質量百分率50質量%に相当する粒子径を中位粒子径として得た。 [Measurement of medium particle size]
The medium particle size of the particles was measured by the following procedure. That is, from the top, the JIS standard sieve has a mesh size of 600 μm, a mesh size of 500 μm, a mesh size of 425 μm, a mesh size of 300 μm, a mesh size of 250 μm, a mesh size of 180 μm, and a mesh size of 150 μm. , And the saucer in that order. 50 g of particles were placed in the best combined sieve and classified according to JIS Z 8815 (1994) using a low-tap shaker (manufactured by Iida Seisakusho Co., Ltd.). After classification, the mass of the particles remaining on each sieve was calculated as a mass percentage with respect to the total amount, and the particle size distribution was obtained. The relationship between the mesh size of the sieve and the integrated value of the mass percentage of the particles remaining on the sieve was plotted on a logarithmic probability paper by integrating the particle size distribution on the sieve in order from the largest particle size. By connecting the plots on the probability paper with a straight line, the particle size corresponding to the cumulative mass percentage of 50% by mass was obtained as the medium particle size.
吸水性樹脂粒子の生理食塩水吸水量は以下の方法で測定した。500mL容のビーカーに、生理食塩水500gを量り取り、マグネチックスターラーバー(8mmφ×30mm、リング無し)で600rpm(r/min)で撹拌させながら、吸水性樹脂粒子2.0gを、ママコが発生しないように分散させた。撹拌させた状態で60分間放置し、吸水性樹脂粒子を十分に膨潤させた。その後、あらかじめ目開き75μm標準篩の質量We(g)を測定しておき、これを用いて、上記ビーカーの内容物をろ過し、篩を水平に対して約30度の傾斜角となるように傾けた状態で、30分間放置することにより余剰の水分をろ別した。膨潤ゲルの入った篩の質量Wf(g)を測定し、以下の式により、生理食塩水の吸水量を求めた。
生理食塩水の吸水量=(Wf-We)/2.0 [Water absorption of saline (g / g)]
The amount of physiological saline absorbed by the water-absorbent resin particles was measured by the following method. Weigh 500 g of physiological saline in a 500 mL beaker and stir with a magnetic stirrer bar (8 mmφ x 30 mm, no ring) at 600 rpm (r / min) to generate 2.0 g of water-absorbent resin particles. Dispersed so as not to. The water-absorbent resin particles were sufficiently swollen by being left to stand for 60 minutes in a stirred state. After that, the mass We (g) of a standard sieve having an opening of 75 μm is measured in advance, and the contents of the beaker are filtered using this so that the sieve has an inclination angle of about 30 degrees with respect to the horizontal. Excess water was filtered off by leaving it in an inclined state for 30 minutes. The mass Wf (g) of the sieve containing the swelling gel was measured, and the amount of water absorbed by the physiological saline was determined by the following formula.
Water absorption of saline = (Wf-We) /2.0
製造例15
目付量38g/m2のエアレイド不織布(Chinasilk(Shanghai)New Material Technology Co.,Ltd.MB0401-T1)を14cm×42cmのサイズに2枚分裁断し、エアレイド不織布―1、2とした。エアレイド不織布―1に14cm×42cmのサイズに裁断した目付量45g/m2のエアスルー不織布(Hualong(Nanjing)製)を載置し、気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用い、不織布の中心部10cm×40cmの範囲に対して6.0gの吸水性樹脂粒子(住友精化株式会社製のアクアキープSA60S、生理食塩水の吸水量60g/g、中位粒子径342μm)を均一に散布させた。 [Manufacturing of water absorption core]
Production example 15
Two air-laid non-woven fabrics (Chinasilk (Shanghai) New Material Technology Co., Ltd. MB0401-T1) having a basis weight of 38 g / m 2 were cut into two pieces having a size of 14 cm × 42 cm to obtain air-laid non-woven fabrics-1 and 2. An air-through non-woven fabric (manufactured by Hualong (Nanjining)) with a grain size of 45 g / m 2 cut into a size of 14 cm x 42 cm is placed on the air-laid non-woven fabric-1 and an air flow type mixer (manufactured by Otec Co., Ltd., pad former) is installed. 6.0 g of water-absorbent resin particles (Aquakeep SA60S manufactured by Sumitomo Seika Chemical Co., Ltd., water absorption of physiological saline 60 g / g, medium particle diameter 342 μm) for a range of 10 cm × 40 cm in the center of the non-woven fabric. Was evenly sprayed.
気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用いて、吸水性樹脂粒子(住友精化株式会社製アクアキープSA60S、生理食塩水の吸水量60g/g、中位粒子径342μm)12.0g及び粉砕パルプ3.0gを空気抄造によって均一混合することにより、40cm×10cmの大きさのシート状の吸収層を作製した。次に、シート状の吸収層と同じ大きさを有する目付量16g/m2の2枚のティッシュで吸収層の上下を挟んだ状態で全体に196kPaの荷重を30秒間加えてプレスすることにより吸水コアを作製した。これを吸水コアBとした。作製した吸水コアBは、2枚のティッシュの間に、吸水性樹脂粒子及び粉砕パルプからなる吸収層が配置されたものである。 Production example 16
Water-absorbent resin particles (Aquakeep SA60S manufactured by Sumitomo Seika Chemical Co., Ltd., water absorption of physiological saline 60 g / g, medium particle diameter 342 μm) using an air flow type mixer (Padformer manufactured by Otec Co., Ltd.) A sheet-shaped absorbent layer having a size of 40 cm × 10 cm was prepared by uniformly mixing 12.0 g and 3.0 g of pulverized pulp by air papermaking. Next, water absorption is performed by applying a load of 196 kPa to the entire surface for 30 seconds with the upper and lower sides of the absorbent layer sandwiched between two sheets of tissue having the same size as the sheet-shaped absorbent layer and having a basis weight of 16 g / m 2. The core was made. This was designated as the water absorption core B. The produced water-absorbing core B has an absorbing layer made of water-absorbing resin particles and crushed pulp arranged between two sheets of tissue.
実施例1
(補助シートの作製)
目付量16g/m2のティッシュを14cm×42cmのサイズに2枚分裁断し、補助シートの上部用シート基材、下部用シート基材とした。下部用シート基材のロール内側面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した後、速やかに気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用いて、下部用シート基材の中心部10cm×40cmの範囲に対し、製造例1にて作製した吸水性樹脂粒子A1.5gを均一に散布させた。上部用シート基材に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した。上部用シート基材の接着剤を塗布した面を下部用シート基材の吸水性樹脂が散布された面に両端を揃えて合わせ重ね、面全体を接着させ、吸水性樹脂が散布されている範囲(10cm×40cm)を切り取り、補助シートを得た。 [Preparation of absorbent articles for testing]
Example 1
(Preparation of auxiliary sheet)
Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 14 cm × 42 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (3M Spray Glue 77 manufactured by 3M Japan Ltd.) to the inner surface of the roll of the lower sheet base material, promptly airflow type mixing device (manufactured by Otec Co., Ltd., pad former) ) Was used to uniformly spray 1.5 g of the water-absorbent resin particles A prepared in Production Example 1 over a range of 10 cm × 40 cm in the center of the lower sheet base material. 0.3 g of an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to the upper sheet base material. The surface coated with the adhesive of the upper sheet base material is overlapped with the surface on which the water-absorbent resin of the lower sheet base material is sprayed, with both ends aligned, and the entire surface is adhered to the area where the water-absorbent resin is sprayed. (10 cm × 40 cm) was cut out to obtain an auxiliary sheet.
得られた補助シートの上部用シート基材上に製造例15にて作製した吸水コアAを載せ、吸収性物品を得た。 (Preparation of absorbent articles for testing)
The water-absorbing core A prepared in Production Example 15 was placed on the upper sheet base material of the obtained auxiliary sheet to obtain an absorbent article.
補助シート用の吸水性樹脂粒子を製造例2にて作製した吸水性樹脂粒子Bに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 2
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles B produced in Production Example 2.
補助シート用の吸水性樹脂粒子を製造例3にて作製した吸水性樹脂粒子Cに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 3
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles C produced in Production Example 3.
補助シート用の吸水性樹脂粒子を製造例4にて作製した吸水性樹脂粒子Dに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 4
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles D produced in Production Example 4.
補助シート用の吸水性樹脂粒子を製造例5にて作製した吸水性樹脂粒子Eに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 5
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles E produced in Production Example 5.
補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 6
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6.
補助シート用の吸水性樹脂粒子を製造例7にて作製した吸水性樹脂粒子Gに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 7
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles G produced in Production Example 7.
補助シート用の吸水性樹脂粒子を製造例8にて作製した吸水性樹脂粒子Hに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 8
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles H produced in Production Example 8.
補助シート用の吸水性樹脂粒子を製造例9にて作製した吸水性樹脂粒子Jに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 9
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles J produced in Production Example 9.
補助シートの上部用シート基材及び下部用シート基材を目付量17g/m2のスパンボンド不織布(Toray Polytech(Nantong)Co.,Ltd.製、商品名:LIVSEN)に変更したこと、並びに補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 10
The upper sheet base material and the lower sheet base material of the auxiliary sheet were changed to spunbonded non-woven fabric (manufactured by Toray Polytech (Nantong) Co., Ltd., trade name: LIVESEN) having a basis weight of 17 g / m 2. An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the sheet were changed to the water-absorbent resin particles F produced in Production Example 6.
補助シートの上部用シート基材及び下部用シート基材を目付量21g/m2のレンゴー・ノンウーブン・プロダクツ株式会社製エアスルー不織布に変更したこと、並びに補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 11
The upper sheet base material and the lower sheet base material of the auxiliary sheet were changed to air-through non-woven fabric manufactured by Rengo Nonwoven Products Co., Ltd. with a grain size of 21 g / m 2, and water-absorbent resin particles for the auxiliary sheet were produced. An absorbent article was obtained in the same manner as in Example 1 except that the particles were changed to the water-absorbent resin particles F produced in 1.
補助シートの上部用シート基材を目付量45g/m2のHualong(Nanjing)社製エアスルー不織布に変更したこと、及び補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 12
The upper sheet base material of the auxiliary sheet was changed to an air-through non-woven fabric manufactured by Hualong (Nanjining) with a grain size of 45 g / m 2, and the water-absorbent resin particles for the auxiliary sheet were prepared in Production Example 6. An absorbent article was obtained in the same manner as in Example 1 except that it was changed to F.
(補助シートの作製)
気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用いて、製造例6の吸水性樹脂粒子F1.5g及び粉砕パルプ1.5gを空気抄造によって均一混合することにより、40cm×10cmの大きさのシート状の樹脂層を作製した。次に、シート状の樹脂層と同じ大きさを有する目付量16g/m2の2枚のティッシュで樹脂層の上下を挟んだ状態で全体に196kPaの荷重を30秒間加えてプレスすることにより、吸水性樹脂粒子及び粉砕パルプからなる樹脂層が、2枚のティッシュの間に配置されている、補助シートを得た。 Example 13
(Preparation of auxiliary sheet)
By using an air flow type mixer (Padformer manufactured by Otec Co., Ltd.) to uniformly mix 1.5 g of the water-absorbent resin particles F and 1.5 g of crushed pulp of Production Example 6 by air papermaking, the size is 40 cm × 10 cm. A sheet-shaped resin layer having a size was prepared. Next, a load of 196 kPa is applied to the entire surface for 30 seconds while the resin layer is sandwiched between two sheets of tissue having the same size as the sheet-shaped resin layer and having a grain size of 16 g / m 2, and pressed. An auxiliary sheet was obtained in which a resin layer composed of water-absorbent resin particles and crushed pulp was arranged between two sheets of tissue.
得られた補助シートの上に製造例15にて作製した吸水コアAを置き、吸収性物品を得た。 (Preparation of absorbent articles for testing)
The water-absorbing core A prepared in Production Example 15 was placed on the obtained auxiliary sheet to obtain an absorbent article.
補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと、吸水性樹脂粒子の使用量を1.0gに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 14
The same as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6 and the amount of the water-absorbent resin particles used was changed to 1.0 g. An absorbent article was obtained.
補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと以外は実施例1と同様にして補助シートを得た。得られた補助シートに製造例16にて作製した吸水コアBを載せ、吸収性物品を得た。 Example 15
An auxiliary sheet was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6. The water-absorbing core B produced in Production Example 16 was placed on the obtained auxiliary sheet to obtain an absorbent article.
補助シート用の吸水性樹脂粒子を製造例6にて作製した吸水性樹脂粒子Fに変更したこと、吸水性樹脂粒子の使用量を0.4gに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Example 16
The same as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles F produced in Production Example 6 and the amount of the water-absorbent resin particles used was changed to 0.4 g. An absorbent article was obtained.
補助シートを用いずに製造例15にて作製した吸水コアAのみを試験用の吸収性物品とした。 Comparative Example 1
Only the water-absorbing core A produced in Production Example 15 without using the auxiliary sheet was used as the absorbent article for the test.
製造例15のエアレイド不織布―2とエアスルー不織布との間に散布する吸水性樹脂粒子の使用量を6.0gから、5.0gに変更したこと以外は製造例15と同様にして、吸水コアを得た。補助シートを用いずに得られた上記吸水コアのみを試験用の吸収性物品とした。 Comparative Example 2
The water-absorbing core was prepared in the same manner as in Production Example 15 except that the amount of the water-absorbent resin particles sprayed between the air-laid non-woven fabric-2 and the air-through non-woven fabric of Production Example 15 was changed from 6.0 g to 5.0 g. Obtained. Only the above-mentioned water-absorbing core obtained without using the auxiliary sheet was used as an absorbent article for testing.
吸水性樹脂粒子を用いなかったこと以外は実施例1と同様にして吸収性物品を得た。 Comparative Example 3
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles were not used.
補助シート用の吸水性樹脂粒子を製造例10にて作製した吸水性樹脂粒子Kに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Comparative Example 4
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles K produced in Production Example 10.
補助シート用の吸水性樹脂粒子を製造例11にて作製した吸水性樹脂粒子Lに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Comparative Example 5
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles L produced in Production Example 11.
補助シート用の吸水性樹脂粒子を製造例12にて作製した吸水性樹脂粒子Mに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Comparative Example 6
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles M produced in Production Example 12.
補助シート用の吸水性樹脂粒子を製造例13にて作製した吸水性樹脂粒子Nに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Comparative Example 7
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles N produced in Production Example 13.
補助シート用の吸水性樹脂粒子を製造例14にて作製した吸水性樹脂粒子Pに変更したこと以外は実施例1と同様にして吸収性物品を得た。 Comparative Example 8
An absorbent article was obtained in the same manner as in Example 1 except that the water-absorbent resin particles for the auxiliary sheet were changed to the water-absorbent resin particles P produced in Production Example 14.
補助シートを用いずに製造例16にて作製した吸収コアのみを試験用の吸収性物品とした。 Comparative Example 9
Only the absorbent core prepared in Production Example 16 without using the auxiliary sheet was used as the absorbent article for the test.
以下の材料を用いて人工尿を調製した。
・イオン交換水:9865.75g
・NaCl:100.0g
・CaCl2・H2O:3.0g
・MgCl2・6H2O:6.0g
・トリトン X-100(1%):25.0g
・食用青色1号(着色用):0.25g [Preparation of artificial urine]
Artificial urine was prepared using the following materials.
-Ion-exchanged water: 9865.75 g
-NaCl: 100.0 g
・ CaCl 2・ H 2 O: 3.0 g
· MgCl 2 · 6H 2 O: 6.0g
-Triton X-100 (1%): 25.0 g
・ Edible blue No. 1 (for coloring): 0.25g
乾粉通液吸液率は、式:乾粉通液吸液率=乾粉通液吸液量(g)/0.2gの吸水性樹脂の人工尿飽和吸液量(g)により算出される。乾粉通液吸液量及び0.2gの人工尿飽和吸液量は以下に示す方法で測定・算出した。 [Measurement of dry powder flow absorption rate]
The dry powder passing liquid absorption rate is calculated by the formula: dry powder passing liquid absorbing rate = dry powder passing liquid absorbing amount (g) / 0.2 g artificial urine saturated liquid absorbing amount (g) of the water-absorbent resin. The dry powder passing liquid absorption amount and the artificial urine saturated liquid absorption amount of 0.2 g were measured and calculated by the methods shown below.
図5は、乾粉通液吸液率の測定方法を示す模式図である。ステンレス製のメッシュ51(目開き50μm)がメッシュ状の底部として接着された、内径60mm、外径69mm、高さ60mmであるアクリル樹脂製の円筒状容器52に、0.2gの吸水性樹脂粒子61aを均一に散布し、容器及び容器内に散布された吸水性樹脂粒子61aの合計質量Wbを測定した。 [Measurement of dry powder flow absorption amount]
FIG. 5 is a schematic view showing a method for measuring the liquid absorption rate of dry powder. 0.2 g of water-absorbent resin particles in a
500mL容のビーカーに、人工尿500gを量り取り、マグネチックスターラーバー(8mmφ×30mm、リング無し)を用いて600rpm(r/min)で撹拌させながら、2.0gの吸水性樹脂粒子を、ママコが発生しないように分散させた。60分間撹拌を継続し、吸水性樹脂粒子を十分に膨潤させた。あらかじめ目開き75μm標準篩の質量Wc(g)を測定しておき、これを用いて、ビーカーの内容物をろ過し、1分間静置することで余剰の水分をろ別した。膨潤ゲルの入った篩の質量Wd(g)を測定し、以下の式により、人工尿飽和吸液量を求めた。
・人工尿飽和吸液量(g/g)=(Wd-Wc)/2.0
・0.2gの人工尿飽和吸液量(g)=0.2×人工尿飽和吸液量(g/g) [Measurement of artificial urine saturated liquid absorption amount of water-absorbent resin particles]
Weigh 500 g of artificial urine into a 500 mL beaker, and stir at 600 rpm (r / min) using a magnetic stirrer bar (8 mmφ x 30 mm, without ring) to add 2.0 g of water-absorbent resin particles to Mamako. Was dispersed so that Stirring was continued for 60 minutes to sufficiently swell the water-absorbent resin particles. The mass Wc (g) of a standard sieve having a mesh size of 75 μm was measured in advance, and the contents of the beaker were filtered using this and allowed to stand for 1 minute to filter out excess water. The mass Wd (g) of the sieve containing the swelling gel was measured, and the artificial urine saturated liquid absorption amount was determined by the following formula.
-Artificial urine saturated liquid absorption (g / g) = (Wd-Wc) /2.0
-0.2 g of artificial urine saturated liquid absorption (g) = 0.2 x artificial urine saturated liquid absorption (g / g)
補助シートの厚みを、精密厚み測定器(尾崎製作所製、ダイヤルシックネスゲージJ-B、測定子:アルミ製φ50mm)を用いて測定した。測定は補助シートの中央部に測定子が接する位置にて行い、3回測定した値を平均したものを補助シートの厚み(mm)とした。 [Auxiliary sheet thickness evaluation]
The thickness of the auxiliary sheet was measured using a precision thickness measuring instrument (manufactured by Ozaki Seisakusho, dial thickness gauge JB, stylus: aluminum φ50 mm). The measurement was performed at a position where the stylus was in contact with the central portion of the auxiliary sheet, and the average of the values measured three times was taken as the thickness (mm) of the auxiliary sheet.
図6は、吸収性物品の液体漏れを評価する装置を示す模式図である。図6に示される装置を用いて、以下の(i),(ii),(iii)及び(iv)の手順により、試験用の吸収性物品100の吸液初期段階の液体漏れ性を評価した。表1に結果を示す。表中の樹脂は吸水性樹脂粒子を表し、gsmはg/m2を表す。 [Evaluation of liquid leakage in the initial stage of liquid absorption]
FIG. 6 is a schematic view showing an apparatus for evaluating liquid leakage of an absorbent article. Using the apparatus shown in FIG. 6, the liquid leakage property at the initial stage of liquid absorption of the
(ii)アクリル樹脂板1を、メカニカルファスナーが接着された主面S1を上方にして、市販の実験設備用の架台41を用いて固定した。このとき、アクリル樹脂板1の長辺が水平面に平行で、アクリル樹脂板1の主面と水平面S0とが45±2度をなすように固定した。固定されたアクリル樹脂板1の主面S1に、試験用の吸収性物品100を、その長辺がアクリル樹脂板1の長辺に対して垂直になる向きで、試験用の吸収性物品100の下端が、アクリル樹脂板1の下端と同じ位置になるように貼り付けた。吸水コア及び補助シートからなる試験用の吸収性物品100は、吸水コアが表側になるようにアクリル樹脂板1上に貼り付けた。落下防止のため、試験用の吸収性物品100の上端をアクリル樹脂板1に粘着テープで固定した。
(iii)試験用の吸収性物品100中の吸収コアの中央から8cm上方を投入点とし、投入点から鉛直上方1cmの位置から、滴下漏斗42(株式会社コスモスビード製 滴下ロート300mL容、先端部の内径が8mm×6mm)を用いて、8mL/秒の速度にて液温25℃に調整した所定量の人工尿45を注入した。吸水性樹脂粒子からなる吸収層を備える吸水コアAを用いたときの人工尿45の注入量は、80mLであり、吸水性樹脂粒子及び粉砕パルプからなる吸収層を備える吸水コアBを用いたときの人工尿45の注入量は120mLであった(表1中、*を付した実施例又は比較例)。
(iv)試験用の吸収性物品100から漏れ出た人工尿は、予め吸収性物品100の下方に設置され、かつ天秤上に配置された金属トレー44内に回収された。回収された人工尿を計量し、人工尿の投入量(g)に対する漏れ出た人工尿の量(g)の割合(%)を算出した。 (I) is a mechanical fastener (3M mechanical fastener hook), vertical 45cm, was cut to the size of the
The (ii) an
(Iii) The loading point is 8 cm above the center of the absorption core in the
(Iv) The artificial urine leaked from the
10, 10A, 10B ... Absorbent layer, 10a ... Water-absorbent resin particles, 10b ... Fiber layer, 20a, 20b ... Core wrap sheet, 21 ... Adhesive, 25a, 25b, 25c ... Core wrap sheet, 26a, 26b ... Adhesive , 30 ... Liquid permeable sheet, 40 ... Liquid permeable sheet, 50 ... Water absorption core, 51 ... Mesh (mesh-like bottom), 52 ... Cylindrical container, 60 ... Auxiliary sheet, 61 ... Resin layer, 61a ... Water absorption Sex resin particles, 61b ... fiber layer, 62a, 62b ... sheet base material, 63a, 63b ... adhesive, 100 ... absorbent article.
Claims (3)
- 吸水コア、該吸水コアによる吸液を補助する補助シート、液体不透過性シート及び液体透過性シートを備え、前記液体不透過性シート、前記補助シート、前記吸水コア及び前記液体透過性シートがこの順に配置されている、吸収性物品であって、
前記補助シートが吸水性樹脂粒子を含む樹脂層を備え、
以下の(1)、(2)、(3)、(4)及び(5)の工程をこの順に含む方法により測定される、前記吸水性樹脂粒子の乾粉通液吸液率が0.25以上1.0以下である、吸収性物品。
(1)メッシュ状の底部を備える内径60mmの円筒状容器内の底面全体にわたり、0.2gの吸水性樹脂粒子を均一に散布し、前記容器及び該容器内に散布された前記吸水性樹脂粒子の合計質量Wb(g)を測定する。
(2)前記吸水性樹脂粒子が散布された前記容器内に液温25℃の人工尿20mLを8mL/秒の一定速度で注入し、前記人工尿の少なくとも一部を前記吸水性樹脂粒子に吸液させて前記容器内で膨潤ゲルを形成させる。
(3)注入開始から30秒後に、前記容器及び該容器内の膨潤ゲルの合計質量Wa(g)を測定する。
(4)Wa(g)-Wb(g)により乾粉通液吸液量(g)を求める。
(5)0.2gの吸水性樹脂粒子の人工尿飽和吸液量(g)に対する乾粉通液吸液量(g)の比として、乾粉通液吸液率(g/g)を得る。 A water absorption core, an auxiliary sheet assisting liquid absorption by the water absorption core, a liquid impermeable sheet and a liquid permeable sheet are provided, and the liquid impermeable sheet, the auxiliary sheet, the water absorption core and the liquid permeable sheet are the same. Absorbent articles arranged in order,
The auxiliary sheet includes a resin layer containing water-absorbent resin particles.
The dry powder passing liquid absorption rate of the water-absorbent resin particles measured by a method including the following steps (1), (2), (3), (4) and (5) in this order is 0.25 or more. Absorbent article, 1.0 or less.
(1) 0.2 g of water-absorbent resin particles are uniformly sprayed over the entire bottom surface of a cylindrical container having an inner diameter of 60 mm having a mesh-like bottom, and the container and the water-absorbent resin particles sprayed in the container. The total mass Wb (g) of the above is measured.
(2) 20 mL of artificial urine having a liquid temperature of 25 ° C. is injected into the container on which the water-absorbent resin particles are sprayed at a constant rate of 8 mL / sec, and at least a part of the artificial urine is absorbed by the water-absorbent resin particles. Let it liquid to form a swollen gel in the container.
(3) 30 seconds after the start of injection, the total mass Wa (g) of the container and the swollen gel in the container is measured.
(4) The dry powder passing liquid absorption amount (g) is determined from Wa (g) -Wb (g).
(5) The dry powder passage liquid absorption rate (g / g) is obtained as the ratio of the dry powder passage liquid absorption amount (g) to the artificial urine saturated liquid absorption amount (g) of 0.2 g of the water-absorbent resin particles. - おむつである、請求項1に記載の吸収性物品。 The absorbent article according to claim 1, which is a diaper.
- 吸水コアを備える吸収性物品において、前記吸水コアの吸液を補助するために用いられる補助シートであって、
吸水性樹脂粒子を含む樹脂層を備え、
以下の(1)、(2)、(3)、(4)及び(5)の工程をこの順に含む方法により測定される、前記吸水性樹脂粒子の乾粉通液吸液率が0.25以上1.0以下である、補助シート。
(1)メッシュ状の底部を備える内径60mmの円筒状容器内の底面全体にわたり、0.2gの吸水性樹脂粒子を均一に散布し、前記容器及び該容器内に散布された前記吸水性樹脂粒子の合計質量Wb(g)を測定する。
(2)前記吸水性樹脂粒子が散布された前記容器内に液温25℃の人工尿20mLを8mL/秒の一定速度で注入し、前記人工尿の少なくとも一部を前記吸水性樹脂粒子に吸液させて前記容器内で膨潤ゲルを形成させる。
(3)注入開始から30秒後に、前記容器及び該容器内の前記膨潤ゲルの合計質量Wa(g)を測定する。
(4)Wa(g)-Wb(g)により乾粉通液吸液量(g)を求める。
(5)0.2gの吸水性樹脂粒子の人工尿飽和吸液量(g)に対する乾粉通液吸液量(g)の比として、乾粉通液吸液率(g/g)を得る。
An auxiliary sheet used to assist the absorption of liquid in the water absorption core in an absorbent article including the water absorption core.
With a resin layer containing water-absorbent resin particles,
The dry powder passing liquid absorption rate of the water-absorbent resin particles measured by a method including the following steps (1), (2), (3), (4) and (5) in this order is 0.25 or more. Auxiliary sheet that is 1.0 or less.
(1) 0.2 g of water-absorbent resin particles are uniformly sprayed over the entire bottom surface of a cylindrical container having an inner diameter of 60 mm having a mesh-like bottom, and the container and the water-absorbent resin particles sprayed in the container. The total mass Wb (g) of the above is measured.
(2) 20 mL of artificial urine having a liquid temperature of 25 ° C. is injected into the container on which the water-absorbent resin particles are sprayed at a constant rate of 8 mL / sec, and at least a part of the artificial urine is absorbed by the water-absorbent resin particles. Let it liquid to form a swollen gel in the container.
(3) 30 seconds after the start of injection, the total mass Wa (g) of the container and the swollen gel in the container is measured.
(4) The dry powder passing liquid absorption amount (g) is determined from Wa (g) -Wb (g).
(5) The dry powder passage liquid absorption rate (g / g) is obtained as the ratio of the dry powder passage liquid absorption amount (g) to the artificial urine saturated liquid absorption amount (g) of 0.2 g of the water-absorbent resin particles.
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JP2014073448A (en) * | 2012-10-03 | 2014-04-24 | Nippon Shokubai Co Ltd | Particulate water absorbent and its manufacturing method |
JP2016112047A (en) * | 2014-12-11 | 2016-06-23 | 株式会社リブドゥコーポレーション | Sheet member for absorptive article and absorptive article |
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