WO2005012369A1 - Procede de fabrication de resine absorbant l'eau - Google Patents

Procede de fabrication de resine absorbant l'eau Download PDF

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Publication number
WO2005012369A1
WO2005012369A1 PCT/JP2004/011284 JP2004011284W WO2005012369A1 WO 2005012369 A1 WO2005012369 A1 WO 2005012369A1 JP 2004011284 W JP2004011284 W JP 2004011284W WO 2005012369 A1 WO2005012369 A1 WO 2005012369A1
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Prior art keywords
water
absorbent resin
weight
polymerization
monomer
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PCT/JP2004/011284
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English (en)
Japanese (ja)
Inventor
Kazuhiro Yoshino
Tomoki Kawakita
Yasuhiro Nawata
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Sumitomo Seika Chemicals Co., Ltd.
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Priority to JP2005512584A priority Critical patent/JPWO2005012369A1/ja
Publication of WO2005012369A1 publication Critical patent/WO2005012369A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/04—Polymerisation in solution
    • C08F2/10—Aqueous solvent
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents

Definitions

  • the present invention relates to a method for producing a water absorbent resin. More specifically, the present invention relates to a method for producing a water-absorbent resin that can be suitably used in the field of sanitary materials such as disposable diapers and sanitary napkins. Light
  • water-absorbent resins have been widely used in sanitary materials such as disposable diapers and sanitary napkins, and industrial materials such as waterproofing agents for cables.
  • water-absorbent resin examples include a hydrolyzate of starch-acrylonitrile graft copolymer, a neutralized product of starch-acrylic acid graft polymer, a saponified product of vinyl acetate-acrylate copolymer, and a polyacrylic acid portion. Neutralized substances and the like are known.
  • these water-absorbing resins have a high water absorption under a pressure higher than the atmospheric pressure (hereinafter referred to as water absorption under pressure), but have a high water absorption under the atmospheric pressure (hereinafter, referred to as “water absorption under pressure”). Water absorption under no pressure) is insufficient. Therefore, when these water-absorbing resins are used in adult diapers and the like, for which needs have been increasing in recent years, the water absorption under no pressure is low, and sufficient absorption performance cannot be exhibited.
  • Examples of a method for producing a water-absorbing agent excellent in water absorption under pressure and water absorption under pressure include, for example, a water-absorbent resin having a lipoxyl group, an inorganic acid or an organic acid which can be dissolved in an aqueous liquid, and lipoxyl.
  • a method of mixing a crosslinking agent capable of reacting with a group is known.
  • the present invention has been made in view of the prior art, and provides a method for producing a water-absorbent resin which has excellent water absorption under no pressure and water absorption under pressure, and can be suitably used for sanitary materials and the like. As an issue.
  • a method for producing a water-absorbent resin having a step of polymerizing a water-soluble ethylenically unsaturated monomer in the presence of a crosslinking agent, wherein the polymerization of the monomer is further carried out by lactic acid and / or A method for producing a water-absorbent resin, which is performed in the presence of a salt thereof,
  • the water absorption under pressure and the water absorption under pressure are both excellent, and the water-absorbing resin which can be suitably used for sanitary materials etc. can be manufactured efficiently.
  • FIG. 1 is a schematic explanatory view of a measuring device X used for measuring the amount of water absorption under pressure.
  • X is a measuring device
  • 1 is an electronic balance
  • 2 is a bottle
  • 3 is an air intake pipe
  • 4 is a conduit
  • 5 is a glass filter
  • 6 is a measuring unit
  • 7 is a computer
  • 8 is saline
  • 9 is water absorption.
  • 60 indicates a cylinder
  • 61 indicates a nylon mesh
  • 62 indicates a weight.
  • the method for producing a water-absorbent resin of the present invention is a method for producing a water-absorbent resin having a step of polymerizing a water-soluble ethylenically unsaturated monomer in the presence of a cross-linking agent. Is performed in the presence of lactic acid and / or a salt thereof. With such a configuration, according to the present invention, a water-absorbent resin excellent in both the water absorption under pressure and the water absorption under pressure can be efficiently produced.
  • water absorption means both the water absorption under no pressure and the water absorption under pressure.
  • Water-soluble in the water-soluble ethylenically unsaturated monomer used in the present invention refers to the property of dissolving the monomer in water, and is independent of the dissolution temperature if it is soluble in water.
  • the monomer is not particularly limited as long as it is a compound having a polymerizable ethylene group.
  • the monomer examples include (meth) acrylic acid [“(meth) acryl J” means “acryl” and “methacryl”. The same applies hereinafter), 2- (meth) acrylamide—2-methylpropanesulfonic acid or their metal salts; (meth) acrylamide, N, N-dimethylacrylamide, 2-hydroxyethyl (meth) acrylate, N-methylol
  • Nonionic monomers such as (meth) acrylamide; amino-containing unsaturated monomers such as getylaminoethyl (meth) acrylate and getylaminopropyl (meth) acrylate; and quaternized products thereof. These may be used alone or in combination of two or more.
  • examples of the alkali metal in the alkali metal salt include lithium, sodium, and potassium, and among them, sodium and / or potassium are preferable from the viewpoint of excellent water absorption and economy.
  • Preferred among the water-soluble ethylenically unsaturated monomers are acrylic acid or an alkali metal salt thereof, methacrylic acid or an alkali metal salt thereof, acrylamide, methacrylamide and the like because of industrial availability.
  • the water-soluble ethylenically unsaturated monomer is preferably used as an aqueous solution.
  • concentration of the water-soluble ethylenically unsaturated monomer in an aqueous solution of a water-soluble ethylenically unsaturated monomer (hereinafter, referred to as a monomer aqueous solution) is preferably from 25% by weight to a saturated concentration.
  • the water used is not particularly limited, and includes tap water, distilled water, ion-exchanged water, and the like.
  • the monomer aqueous solution may be used after neutralizing the acid group with an alkali metal.
  • the degree of neutralization by the alkali metal is to increase the osmotic pressure of the resulting water-absorbent resin and increase the water absorption rate, while preventing the safety and other problems from being caused by the presence of excess metal. Therefore, it is preferably 10 to 100 mol% of the acid groups of the water-soluble ethylenically unsaturated monomer before neutralization.
  • the alkali metal include lithium, sodium, potassium, and the like. Of these, sodium and Z or potassium are preferred.
  • the neutralization of the acid group can be performed, for example, by dropping an aqueous solution of a compound containing an alkali metal such as sodium hydroxide, potassium hydroxide or the like into the monomer aqueous solution and mixing.
  • concentration of the alkali metal-containing compound in the aqueous solution is not particularly limited, but is usually about 20 to 50% by weight.
  • the monomer some water-soluble monomers other than the water-soluble ethylenically unsaturated monomer may be used as long as the desired effects of the present invention are not inhibited. Such a water-soluble monomer can be used, for example, by mixing it with the monomer aqueous solution.
  • the method for polymerizing the monomer is not particularly limited, and examples thereof include a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method.
  • a reverse phase suspension polymerization method from the viewpoints of securing the water absorbing performance of the obtained water-absorbing resin and the ease of controlling the polymerization reaction, A liquid polymerization method or a reversed phase suspension polymerization method is preferable, and a reversed phase suspension polymerization method is particularly preferable.
  • JP-A-56-131160 For details of these polymerization methods, see, for example, JP-A-56-131160.
  • an aqueous monomer solution is dispersed in a hydrocarbon-based solvent containing a surfactant and / or a polymer protective colloid, and a water-soluble radical polymerization initiator is used in the presence of a crosslinking agent.
  • the polymerization of the water-soluble ethylenically unsaturated monomer is carried out.
  • the polymerization of the monomer is carried out in the presence of lactic acid and / or a salt thereof.
  • the reaction system may further include other components such as a compound containing a transition metal and a chain transfer agent.
  • the surfactant, polymer protective colloid, crosslinking agent, hydrocarbon-based solvent, water-soluble radical polymerization initiator, and other components used in the polymerization reaction are not particularly limited, and may be reversed phase. What is usually used may be used in the suspension polymerization method.
  • the surfactant used in the present invention include nonionic surfactants such as sorbitan fatty acid ester, polyglycerin fatty acid ester, sucrose fatty acid ester, sorbitol fatty acid ester, and polyoxetylene alkylphenyl ether.
  • Anionic surfactants such as fatty acid salts, alkyl benzene sulfonates, alkyl methyl taurates, polyoxyethylene alkyl phenyl ether sulfates, and polyoxetylene alkyl ether sulfonates.
  • sorbitan fatty acid esters, polyglycerin fatty acid esters, and sucrose fatty acid esters are preferred.
  • polymer protective colloid used in the present invention examples include, for example, ethyl cellulose, ethyl hydroxyethyl cellulose, polyethylene oxide, maleic anhydride polyethylene, maleic anhydride polybutadiene, maleic anhydride EPDM (ethyl acetate). Ren / propylene Z Genno Yuichi Polymer).
  • the amount of the surfactant and the protective colloid is preferably 0.1 to 5 parts by weight, preferably 0.2 to 3 parts by weight, per 100 parts by weight of the aqueous solution of the water-soluble ethylenically unsaturated monomer. Parts are more preferred. When both are used, the mixing ratio of both is not particularly limited.
  • water-soluble radical polymerization initiator examples include persulfates such as potassium persulfate, ammonium persulfate, and sodium persulfate; benzoyl peroxide; Organic peroxides such as oxide; hydrogen peroxide; and azo compounds such as 2,2'-azobis (2-amidinopropane) dihydrochloride. Further, a water-soluble radical polymerization initiator and a sulfite or the like can be used in combination to be used as a redox polymerization initiator.
  • potassium persulfate ammonium persulfate, sodium persulfate, benzoyl peroxide and 2,2′-azobis (2-amidinopropane) are preferable from the viewpoint of easy access and good storage stability.
  • Hydrochloride is preferred.
  • the amount of the water-soluble radical polymerization initiator is usually 0.000 to 1 mol of the water-soluble ethylenically unsaturated monomer from the viewpoint of shortening the polymerization reaction time and preventing a rapid polymerization reaction. 5 to 0.01 mole is preferred.
  • hydrocarbon solvent examples include aliphatic hydrocarbons such as n-hexane, n-heptane, and lignin; alicyclic hydrocarbons such as cyclopentane, methylcyclopentane, cyclohexane, and methylcyclohexane. Hydrogen; and aromatic hydrocarbons such as benzene, toluene, and xylene.
  • aliphatic hydrocarbons such as n-hexane, n-heptane, and lignin
  • alicyclic hydrocarbons such as cyclopentane, methylcyclopentane, cyclohexane, and methylcyclohexane. Hydrogen
  • aromatic hydrocarbons such as benzene, toluene, and xylene.
  • n-hexane, n-heptane, and cyclohexane are preferable because they are easily available industrially, have stable quality, and are inexpensive.
  • the amount of the hydrocarbon solvent is usually 50 to 6 with respect to 100 parts by weight of the water-soluble ethylenically unsaturated monomer from the viewpoint of removing the heat of polymerization and making it easier to control the polymerization temperature. 100 parts by weight is preferable, and 100 to 550 parts by weight is more preferable.
  • the crosslinking agent used in the present invention include di- or tri (meth) acrylic polyols such as ethylene glycol, propylene glycol, trimethylolpropane, glycerin, polyoxyethylene daricol, polyoxypropylene glycol, and polyglycerin.
  • Acid esters unsaturated polyesters obtained by reacting the polyols with unsaturated acids such as maleic acid and fumaric acid; bisacrylamides such as N, N, -methylenebisacrylamide; polyepoxides and Di- or tri (meth) acrylates obtained by reacting acrylic acid; polyisocyanates such as tolylene diisocyanate, hexamethylene diisocyanate and hydroxyethyl (meth) acrylate To obtain (Meth) acrylic acid rubamyl esters; arylated starch, arylated cellulose, diallyl phthalate, N, N ', N''-polymerizable unsaturated groups such as triallyl isocyanate, divinylbenzene, etc.
  • unsaturated polyesters obtained by reacting the polyols with unsaturated acids such as maleic acid and fumaric acid
  • bisacrylamides such as N, N, -methylenebisacrylamide
  • the amount of the cross-linking agent is determined per 1 mol of the water-soluble ethylenically unsaturated monomer so that the obtained polymer is suppressed in water-soluble properties by moderate cross-linking and exhibits a sufficient water absorption. , 0.001 to 0.01 mole.
  • Examples of the lactic acid and / or its salt used in the present invention include lactic acid, silver lactate, magnesium lactate, calcium lactate, sodium lactate, potassium lactate and the like.
  • lactic acid is preferably used because it is industrially easily available and inexpensive.
  • Lactic acid and z or a salt thereof are used in an amount of preferably 0.0001 to 0.1 mol, more preferably 0.0001, based on 1 mol of the water-soluble ethylenically unsaturated monomer. To 0.05 mol, more preferably 0.001 to 0.02 mol.
  • the amount of lactic acid and / or its salt is 0.0001 mol or more, the effect of adding lactic acid and / or Z or its salt is sufficiently obtained, while the amount of lactic acid and / or Z or its salt is reduced.
  • the amount is 0.1 mol or less, a resin excellent in both the water absorption under no pressure and the water absorption under pressure is preferably obtained.
  • a hydrocarbon-based solvent including the monomer aqueous solution, a surfactant and a polymer or a polymer protective colloid, a water-soluble radical polymerization initiator, and the like, lactic acid and / or a salt thereof, a crosslinking agent, and other components as required.
  • the mixture is heated under stirring and reverse suspension polymerization is carried out in a water-in-oil system.
  • the order of addition of each component can be appropriately adjusted and is not particularly limited.
  • a surfactant and / or a polymer protective colloid and a hydrocarbon solvent, a water-soluble radical polymerization initiator, and lactic acid it is preferable that the monomer aqueous solution is mixed with Z and / or Z or a salt thereof, a cross-linking agent, and if necessary, other components and the aqueous monomer solution in advance, and the resulting mixed solutions are mixed to initiate polymerization.
  • a multi-stage polymerization method in which a monomer aqueous solution is divided and added in plural times may be used.
  • the polymerization of the water-soluble ethylenically unsaturated monomer is preferably performed by a multi-stage polymerization method from the viewpoint that the average particle size and the amount of water absorption of the obtained water-absorbent resin are easily controlled.
  • the preferred use amount range of each component is based on the total amount of each component used in each stage.
  • the reaction temperature of the polymerization reaction varies depending on the water-soluble radical polymerization initiator used, but the polymerization proceeds quickly, shortening the polymerization time, improving economic efficiency and easily removing the heat of polymerization.
  • the temperature is preferably from 20 to 110 ° C, more preferably from 40 to 90, and still more preferably from 40 to 8 Ot :.
  • the reaction time is usually preferably between 0.5 and 4 hours.
  • the termination of the polymerization reaction can be confirmed, for example, by confirming that the temperature rise in the reaction system has stopped. to this Thus, the water-absorbing resin is usually obtained in a state of a hydrogel.
  • the obtained water-containing gel is dried using, for example, a reduced-pressure drier, a hot-air drier, or the like, to obtain the water-absorbent resin of the present invention.
  • the shape of the obtained water-absorbing resin is not particularly limited, but from the viewpoint of improving the water-absorbing performance, the average particle size of the resin is preferably from 200 to 600 im.
  • the average particle size can be measured, for example, by a method of sieving with a low tap sieve vibrator.
  • the mechanism by which a water-absorbent resin obtained by polymerizing a water-soluble ethylenically unsaturated monomer in the presence of lactic acid and / or a salt thereof is excellent in both water absorption under pressure and water absorption under pressure
  • a water-absorbent resin having excellent water absorption under pressure it is necessary to increase the amount of the crosslinking agent to increase the crosslinking density. The water absorption of the aqueous resin under no pressure is reduced.
  • the crosslinking density can be appropriately increased without increasing the amount of the cross-linking agent to be used. It is presumed that a water-absorbent resin having excellent water absorption under pressure can be obtained.
  • the effect of lactic acid and / or Z or its salt on the microstructure of the water-absorbent resin is not yet known, and it is difficult to define the resin by its structure.
  • the water absorption under pressure and the water absorption under pressure of the obtained water-absorbent resin are clearly superior to those of the conventional one.
  • post-crosslinking treatment surface cross-linking treatment
  • a crosslinking agent containing two or more functional groups having reactivity with the lipoxyl group is performed using gel. It is preferable from the viewpoint of improving strength and water absorption under pressure.
  • Any post-crosslinking agent may be used as long as it can react with the hydroxyl group in the water-absorbing resin.
  • the same cross-linking agent as described above can be used.
  • the amount of the post-crosslinking agent to be used depends on the amount of water absorption under pressure although it varies depending on the type of the crosslinking agent, it is usually preferably 0.005 to 7 parts by weight, more preferably 0.005 to 5 parts by weight, and still more preferably 100 parts by weight of the water-soluble ethylenically unsaturated monomer. 0.01 to 2 parts by weight, particularly preferably 0.01 to 1 part by weight.
  • the amount of the post-crosslinking agent is 0.005 parts by weight or more based on 100 parts by weight of the water-soluble ethylenically unsaturated monomer, the crosslinking density near the surface of the water-absorbent resin can be sufficiently increased, On the other hand, if the amount is 7 parts by weight or less, the amount of the crosslinking agent used is appropriate.
  • the post-crosslinking time of the water-absorbent resin by the post-crosslinking agent may be any time after the completion of the polymerization reaction of the water-soluble ethylenically unsaturated monomer, and is not particularly limited. From the viewpoint of easy control of the water absorption, it is preferable to perform post-crosslinking when the water content of the water-absorbent resin is 5 to 45% by weight.
  • the water content (% by weight) of the water-absorbent resin was determined by measuring the weight a (g) of the water-containing gel after the polymerization reaction and before drying, and the weight b (g) after drying at 105 at 2 hours. The following formula: a (g) one b (g)
  • the post-crosslinking treatment of the water-absorbent resin with the post-crosslinking agent is carried out, for example, by directly adding the post-crosslinking agent after the polymerization reaction of the water-soluble ethylenically unsaturated monomer to powder or an aqueous solution of about 0.5 to 50% by weight It can be carried out by adding to the water-absorbent resin in the form and reacting them at 50 to 150 ° for about 0.5 to 8 hours.
  • the water-absorbing resin of the present invention can be used by being mixed with, for example, a gel stabilizer, a metal chelating agent, silica and the like.
  • the resin may be used according to a known method.
  • granulation or molding may be performed before use.
  • the water-absorbing resin obtained as described above, particularly the post-crosslinked water-absorbing resin is a water-absorbing resin having excellent water absorption under no pressure and water absorption under pressure.
  • a water-absorbing resin is included in the present invention.
  • hygienic materials such as disposable diapers and sanitary napkins, and industrial materials such as a waterproofing agent for cables, etc., which are very excellent in water absorbing ability, can be obtained.
  • the water-absorbent resin of the present invention is suitably used, among others, for producing sanitary materials.
  • the present invention also provides such a sanitary material.
  • the sanitary material and the like can be produced using the water-absorbent resin of the present invention according to a known method (for example, US Pat. No. 5,147,443, Japanese Patent Application Laid-Open No. 5-200006). No. 8).
  • the amount of the resin to be used is not particularly limited, and may be an amount capable of obtaining a desired effect according to the application.
  • each resin was prepared by a reverse phase suspension polymerization method.
  • Example 1 each resin was prepared by a reverse phase suspension polymerization method.
  • n-heptane 340 g sucrose fatty acid ester (Mitsubishi 0.92 g of S-370) was added, and the mixture was dispersed, heated and dissolved, and then cooled to 55 ° C.
  • This monomer aqueous solution was added and dispersed in the above-mentioned five-necked cylindrical round-bottom flask under stirring with stirring, and the system was sufficiently purged with nitrogen, and then heated, and the bath temperature was maintained at 70 ° C. Then, after the first-stage polymerization reaction was performed for 1 hour, one polymerization slurry solution was cooled to room temperature.
  • the inside of the system was sufficiently replaced with nitrogen again, and the temperature was raised.
  • the bath temperature was maintained at 7 Ot: The polymerization reaction of the eyes was performed for 2 hours.
  • the mixture was heated in an oil bath at 120 ° C., and only 260 g of water was removed from the system by azeotropic distillation to obtain a gel.
  • the water content of the obtained gel was 30% by weight.
  • the average particle size of the water-absorbent resin is the integrated weight obtained by sequentially integrating the weight of the water-absorbent resin remaining on each sieve when the water-absorbent resin is classified by a sieve, This corresponds to the sieve opening when it reaches 50% by weight of the total weight.
  • the particle diameter is calculated by the following formula: Average particle diameter (; X (D—B) + B.
  • A is the value obtained when the integrated value is obtained when the integrated weight is less than 50% by weight and the integrated value at the time closest to 50% by weight is calculated.
  • the integrated value (g), and B is the opening m) of the sieve at the time when the integrated value was obtained.
  • C is the value obtained by sequentially calculating the weight from the larger particle size and obtaining the integrated value at the time when the integrated weight is 50% by weight or more and closest to 50% by weight.
  • g) is the sieve opening ( ⁇ m) at the time when the integrated value was obtained.
  • Example 1 the amount of lactic acid in the aqueous monomer solution for the first-stage polymerization was 0.460 g (5.10 mmol), and the amount of lactic acid in the aqueous monomer solution for the second-stage polymerization was 20.1 g of a water-absorbent resin was obtained in the same manner as in Example 1 except that the weight was changed to 0.590 g (6.58 mmo 1). The average particle size of the resin was 372 m.
  • Example 1 the amount of lactic acid in the aqueous monomer solution for the first stage polymerization was 0.230 g (2.55 mmo 1), and the amount of lactic acid in the aqueous monomer solution for the second stage polymerization was Of water-absorbent resin 2 in the same manner as in Example 1 except that the amount of water-absorbent resin 2 was changed to 0.295 g (3.29 mmo 1). 18.2 g were obtained. The average particle size of the resin was 360 m. Comparative Example 1
  • a 50 OmL Erlenmeyer flask was charged with 92 g (1.02 mol) of an 80% by weight aqueous solution of acrylic acid. While cooling from the outside, 102.2 g (0.76 mol) of a 30% by weight aqueous sodium hydroxide solution was added dropwise to neutralize 75 mol% of acrylic acid. In addition, 50.2 g of water, 0.1 llg (0.4 lmmo 1) of potassium persulfate as a water-soluble radical polymerization initiator, and 8.3 mg (0.047 mmo 1) of ethylene glycol diglycidyl ether as a cross-linking agent were added. This was added to prepare a monomer aqueous solution for the first-stage polymerization.
  • This monomer aqueous solution was added and dispersed in the above-mentioned five-necked cylindrical round-bottom flask under stirring with stirring, and the system was sufficiently purged with nitrogen, and then heated, and the bath temperature was maintained at 70 ° C. Then, after performing the first-stage polymerization reaction for 1 hour, one polymerization slurry solution was cooled to room temperature.
  • the water-absorbent resins obtained in the above Examples and Comparative Examples were evaluated by the following methods. The measurement of the water absorption of the water-absorbing resin was performed at room temperature.
  • the water absorption of the water-absorbent resin under no pressure was determined as the water absorption of physiological saline by the resin under atmospheric pressure, and the water-absorbent resins obtained in the above Examples and Comparative Examples were compared.
  • the water absorption under pressure of the water-absorbent resin was determined as the water absorption of physiological saline by the resin under a pressure of 2.07 kPa, and the water-absorbent resins obtained in the above Examples and Comparative Examples were compared. .
  • the amount of water absorption under pressure of the water-absorbent resin was measured using a measuring device X shown in FIG.
  • the measuring device X shown in FIG. 1 is composed of an electronic balance 1, a bottle 2 placed on the electronic balance 1, an air suction pipe 3, a conduit 4, a glass filter 1 and a glass filter 1. 5 and a measuring unit 6 placed on it.
  • the electronic balance 1 is connected to a computer 7 so that the weight change can be recorded in seconds or minutes.
  • the bottle 2 holds a physiological saline solution 8 therein, and has an air suction pipe 3 inserted into an opening at the top, while a conduit 4 is attached to the body.
  • the lower end of the air suction pipe 3 is immersed in a physiological saline solution 8.
  • the diameter of the glass filter 5 is 25 mm.
  • a glass filter No. 1 pore size: 100 to 160 ⁇ of the Mutual Physical and Chemical Glass Laboratory was used.
  • Bottle 2 and glass filter 5 are connected to each other by conduit 4.
  • the glass filter 5 is fixed at a position slightly higher than the lower end of the air suction pipe 3.
  • the measuring section 6 has a cylinder 60, a nylon mesh 61 adhered to the bottom of the cylinder 60, and a weight 62 having a diameter of 19 mm and a weight of 59.8 g.
  • the inner diameter of the cylinder 60 is 20 mm.
  • the nylon mesh 61 is formed in a 200 mesh (mesh size: 75 m). Then, a predetermined amount of the water-absorbing resin 9 is evenly spread on the nylon mesh 61.
  • the measuring device X having such a configuration, first, a predetermined amount of the physiological saline 8 and the air suction pipe 3 are put into the bottle 2 to prepare for the measurement. Next, 0.10 g of the water-absorbent resin 9 is evenly spread on the nylon mesh 61 of the cylinder 60, and the weight 62 is placed on the water-absorbent resin 9. The measuring unit 6 is placed on the glass filter 5 so that the center of the measuring unit 6 is aligned with the center of the glass filter 5.
  • the reduced weight of the physiological saline 8 in the bottle 2 (the physiological saline absorbed by the water-absorbing resin 9) continues from the time when the water absorption is started.
  • the weight of water 8) Wc (g) was recorded on the computer 7 in seconds based on the value obtained from the electronic balance 1.
  • the water absorption under pressure of the water-absorbent resin 9 after a lapse of 60 minutes from the start of water absorption was determined by dividing the weight Wc (g) after the lapse of 60 minutes by the weight of the water-absorbent resin 9 (0.10 g).
  • Table 1 summarizes the evaluation results obtained by the above methods (1) and (2).
  • the present invention provides a method for producing a water-absorbent resin that can be suitably used in the field of sanitary materials such as disposable diapers and sanitary napkins.

Abstract

L'invention concerne un procédé de fabrication d'une résine absorbant l'eau, consistant à polymériser un monomère éthylénique soluble dans l'eau, en présence d'un agent réticulant. Ledit procédé est caractérisé en ce que la polymérisation du monomère est réalisée en présence d'acide lactique et/ou d'un sel d'acide lactique. L'invention concerne également une résine absorbant l'eau obtenue au moyen du procédé selon l'invention, ainsi qu'un article hygiénique faisant intervenir ladite résine absorbant l'eau.
PCT/JP2004/011284 2003-08-04 2004-07-30 Procede de fabrication de resine absorbant l'eau WO2005012369A1 (fr)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007126003A1 (fr) * 2006-04-27 2007-11-08 Sumitomo Seika Chemicals Co., Ltd. Procédé de production de résine absorbant l'eau
WO2008026772A1 (fr) 2006-08-31 2008-03-06 Nippon Shokubai Co., Ltd. Agent particulaire hydro-absorbant et son procédé de production
WO2009005114A1 (fr) 2007-07-04 2009-01-08 Nippon Shokubai Co., Ltd. Agent particulaire hydro-absorbant et son procédé de production
US20110224381A1 (en) * 2010-03-15 2011-09-15 Basf Se Process for Producing Water Absorbing Polymer Particles with Improved Color stability
WO2013155296A1 (fr) * 2012-04-11 2013-10-17 The Procter & Gamble Company Poly(acide acrylique) produit à partir d'acide acrylique bio-ressourcé et ses dérivés
WO2015108113A1 (fr) * 2014-01-16 2015-07-23 日立化成株式会社 Procédé de production de liquide de polissage, et procédé de polissage
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US9630901B2 (en) 2012-04-11 2017-04-25 The Procter & Gamble Company Poly(acrylic acid) from bio-based acrylic acid and its derivatives
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WO2007126002A1 (fr) * 2006-04-27 2007-11-08 Sumitomo Seika Chemicals Co., Ltd. Procédé de production de résine hydro-absorbable
US9074022B2 (en) 2006-04-27 2015-07-07 Sumitomo Seika Chemicals Co., Ltd. Process for production of water-absorbent resin
WO2007126003A1 (fr) * 2006-04-27 2007-11-08 Sumitomo Seika Chemicals Co., Ltd. Procédé de production de résine absorbant l'eau
JP5378790B2 (ja) * 2006-04-27 2013-12-25 住友精化株式会社 吸水性樹脂の製造方法
US8822373B2 (en) 2006-08-31 2014-09-02 Nippon Shokubai Co., Ltd Particulate water absorbing agent and production method thereof
WO2008026772A1 (fr) 2006-08-31 2008-03-06 Nippon Shokubai Co., Ltd. Agent particulaire hydro-absorbant et son procédé de production
JP2010502768A (ja) * 2006-08-31 2010-01-28 株式会社日本触媒 粒子状吸水剤およびその製造方法
EP2057228A1 (fr) * 2006-08-31 2009-05-13 Nippon Shokubai Co., Ltd. Agent particulaire hydro-absorbant et son procédé de production
EP2057228A4 (fr) * 2006-08-31 2010-03-17 Nippon Catalytic Chem Ind Agent particulaire hydro-absorbant et son procédé de production
WO2009005114A1 (fr) 2007-07-04 2009-01-08 Nippon Shokubai Co., Ltd. Agent particulaire hydro-absorbant et son procédé de production
US9006134B2 (en) 2007-07-04 2015-04-14 Nippon Shokubai Co., Ltd. Particulate water absorbing agent and manufacturing method of same
US20110224381A1 (en) * 2010-03-15 2011-09-15 Basf Se Process for Producing Water Absorbing Polymer Particles with Improved Color stability
US8703876B2 (en) * 2010-03-15 2014-04-22 Basf Se Process for producing water absorbing polymer particles with improved color stability
US9132413B2 (en) 2010-07-28 2015-09-15 Sumitomo Seika Chemicals Co., Ltd. Method for producing a water-absorbent resin
JP2015520253A (ja) * 2012-04-11 2015-07-16 ザ プロクター アンド ギャンブルカンパニー バイオベースアクリル酸及びその誘導体由来のポリ（アクリル酸）
CN104204004A (zh) * 2012-04-11 2014-12-10 宝洁公司 得自生物基丙烯酸及其衍生物的聚(丙烯酸)
WO2013155296A1 (fr) * 2012-04-11 2013-10-17 The Procter & Gamble Company Poly(acide acrylique) produit à partir d'acide acrylique bio-ressourcé et ses dérivés
RU2606124C1 (ru) * 2012-04-11 2017-01-10 Дзе Проктер Энд Гэмбл Компани Полиакриловая кислота на основе полученной из биологического сырья акриловой кислоты и ее производных
US9630901B2 (en) 2012-04-11 2017-04-25 The Procter & Gamble Company Poly(acrylic acid) from bio-based acrylic acid and its derivatives
JP2017206712A (ja) * 2012-04-11 2017-11-24 ザ プロクター アンド ギャンブル カンパニー バイオベースアクリル酸及びその誘導体由来のポリ（アクリル酸）
US10344108B2 (en) 2012-04-11 2019-07-09 The Procter & Gamble Company Poly(acrylic acid) from bio-based acrylic acid and its derivatives
WO2015108113A1 (fr) * 2014-01-16 2015-07-23 日立化成株式会社 Procédé de production de liquide de polissage, et procédé de polissage
WO2017170604A1 (fr) * 2016-03-28 2017-10-05 株式会社日本触媒 Procédé de fabrication d'agent d'absorption d'eau
CN109310984A (zh) * 2016-03-28 2019-02-05 株式会社日本触媒 吸水剂的制造方法
JPWO2017170604A1 (ja) * 2016-03-28 2019-02-28 株式会社日本触媒 吸水剤の製造方法
US11224857B2 (en) 2016-03-28 2022-01-18 Nippon Shokubai Co., Ltd. Method for manufacturing water absorbing agent

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