Source: https://patents.google.com/patent/TWI278480B/en
Timestamp: 2019-11-19 19:29:48
Document Index: 742056990

Matched Legal Cases: ['art 6', 'in fine', 'art. 0', 'art 5', 'ART 250', 'Application No. 89']

2007-04-11 Publication of TWI278480B publication Critical patent/TWI278480B/en
The present invention provides a water-absorbent resin composition which contains an aminoacetic chelating agent and is excellent in the urine resistance, wherein the water-absorbent resin composition is excellent further in the light resistance and becomes little colored and might have deodorizability. A water-absorbent resin composition, which comprises a water-absorbent resin and an aminoacetic chelating agent, wherein the mixing ratio of the aminoacetic chelating agent in the water-absorbent resin composition is not less than 10 ppm of the water-absorbent resin, and wherein the total content of nitrilotriacetic acid and its salt in the water-absorbent resin composition is not more than 1 ppm of the water-absorbent resin composition.
1278480 A7 __ B7 V. INSTRUCTION DESCRIPTION (彳) A TECHNICAL FIELD The present invention relates to a water-absorbent resin composition. In particular, the present invention relates to a water-absorbent resin composition in which the water-absorbent resin composition has excellent urine resistance and light resistance, and becomes extremely discolored. Further, the present invention relates to a water-absorbent resin composition which also has excellent deodorizing properties. B. Technical Background In recent years, water-absorbent resins have been widely used as ingredients for sanitary materials, such as disposable diapers, sanitary napkins, and incontinence pads, which are intended to cause water-absorbent resins for absorbing body fluids such as Urine and menstrual blood. For the above water-absorbent resin, the following are known examples: partially neutralized and crosslinked poly(acrylic acid); hydrolyzed starch-acrylonitrile graft polymer; neutralized starch-acrylic graft polymer; a saponified vinyl acetate-acrylate copolymer; a crosslinked polymer of carboxymethylcellulose; a copolymer of hydrolyzed acrylonitrile or acrylamide, or a crosslinked polymer of such a hydrolyzed copolymer; a crosslinked polymer of a cationic monomer; a crosslinked copolymer of isobutylene-maleic acid; and a copolymer of crosslinked 2-propanylamino-2-methylpropanesulfonic acid-acrylic acid. A problem has been pointed out so far. The problem is that when the water-absorbent resin is used as an absorbent structure of a disposable diaper, the water-absorbent resin will deteriorate with time, and its liquid permeability or gel strength will become low, causing urine to be used by itself. The disposable diaper leaked. The deterioration of the water-absorbent resin due to urine is caused by a very small amount of metal ions and L-ascorbic acid contained in the urine. Thus, the paper size has been applied to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) (please read the notes on the back and fill in the ^54 page). Order --------- Line
Ministry of Economic Affairs, Intellectual Property Bureau, Staff Consumer Cooperatives, Printing 1278480 A7 Ministry of Economic Affairs, Intellectual Property Bureau, Staff Consumer Cooperatives, Printing B7__ V. Inventions (2) A technique in which a so-called chelating agent is added to a water-absorbent resin to remove metal ions. Thereby improving the urine resistance of the water absorbent resin. Known examples of the chelating agent include an aminoacetic acid chelating agent such as sodium diethylenetriaminepentaacetate and sodium tris-ethyltetraamine hexaacetate (JP-A-246674/1999, EP 940148A). From the structure of the aminoacetic acid chelating agent, it is expected that the aminoacetic acid chelating agent can not only improve the urine resistance, but also enhance the light resistance of the water absorbent resin. However, previous techniques have only improved urine resistance and, for photosensitivity, provide the same results as those without the addition of an aminoacetic acid chelating agent. On the other hand, the water-absorbent resin is required to have little discoloration with time, and it is considered that the water-absorbent resin is mainly used for sanitary materials (E P 942014). In addition, he is also required to reduce the emission of a disgusting odor, for example, when the water-absorbent resin absorbs urine (USP 5,078,992, JP-A-085082/1997). The first item of the invention provides a water-absorbent resin composition containing an aminoacetic acid chelating agent having excellent urine resistance, wherein the water-absorbent resin composition further has excellent light resistance. The second item of the present invention provides a water-absorbent resin composition which becomes extremely discolored, and further, has little bad odor in use. B. Revelation of the Invention The inventors of the present invention can solve the above problems by diligently researching the results, and have found that (please read the notes on the back side and then fill in the pages) and set the &lt;------- line
This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing ____Β7_5, invention description (3) A reason for not improving light resistance Although the aminoacetic acid chelating agent added in the prior art is nitrogen triacetic acid and/or a salt thereof (hereinafter, 'for the sake of simplicity, the two may collectively be referred to as "nitrogen triacetic acid (salt))" The aminoacetic acid chelating agent becomes an impurity at a concentration of not less than several parts by weight (generally, from about 5 to about 15% by weight). Nitrogen triacetate (salt) is also a substance that may cause anxiety and may be carcinogenic (in the case of I A R C is 2B). Therefore, from the viewpoint of safety, it is considered that the content of the water-absorbent resin composition for contacting the human body such as a disposable diaper must be as low as possible. Aminoacetic acid chelating agents are generally prepared by a process which comprises the steps of reacting aqueous ammonia with ethylidene dichloride or cycloethylimine to form a product such as di-ethyltriamine or tri-ethyltetramine, and This product is then reacted with chloroacetic acid and an alkaline agent such as sodium hydroxide. However, it is considered that unreacted ammonia is retained in the above-mentioned products such as di-ethyltriamine or tri-ethyltetramine, and thus reacts with chloroacetic acid to form nitrogen triacetate (salt) to form impurities. It has been confirmed from the experimental results of the inventors of the present invention that it has been found that the total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition needs to be reduced to not more than 1 ppm, preferably not more than 0. 5 ppm, more preferably No more than 0 · lppm (herein, unless otherwise noted, "ppm" is a water-absorbent resin composition), which is considered to increase light resistance, and further, if it is nitrogen in the water-absorbent resin composition The total content of glycine triacetate (salt) is lowered to this extent, and the discoloration of the water-absorbent resin composition is also extremely small. However, if an attempt is made to reduce the total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition, by simply reducing the mixing ratio of the aminoacetic acid chelating agent, it is possible to read the back of the back-up note.
Page I Scheduled paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) A7 1278480 ____B7__ V. Invention description (4) Enhances light resistance, but on the other hand, urine resistance is extremely degraded, That is, it becomes difficult to maintain or enhance urine resistance by adding a chelating agent. As a result of the experiment by the inventors of the present invention, it has been found that the mixing ratio of the aminoacetic acid chelating agent in the water-absorbent resin composition must be limited to not less than 10 ppm, more preferably not less than 20 ppm. Resin, consider maintaining or improving urine resistance. From the above, it has been found that a water-absorbent resin composition which not only has excellent urine resistance, is photo-resistant, and, in addition, becomes extremely discolored, if the aminoacetic acid chelating agent in the water-absorbent resin composition The mixing ratio is limited to not less than 10 P pm of the water-absorbent resin and further, if the total content of the nitrogen triacetic acid (salt) in the water-absorbent resin composition is limited to not more than 1 ppm, preferably not More than 0 · 5 ppm, more preferably no more than 0. 1 PP m of the water-absorbent resin composition. Thus, the present invention has been completed. The inventors of the present invention further diligently investigated ways to reduce the total content of nitrogen triacetic acid (salt) in the aminoacetic acid chelating agent to enhance the above effects, in other words, to limit the mixing ratio of the aminoacetic acid chelating agent in the water absorbent resin composition. Up to not less than 10 ppm of the water-absorbent resin, and further limited to the total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition to not more than 1 P pm of the water-absorbent resin composition . As a result, it has been found that when the aminoacetic acid chelating agent and the nitrogen triacetic acid are in the form of a salt (-COOX (X: for example, an alkali metal)), both have high water solubility and thus are difficult to separate from each other, but when both are in acid form (a COOH), the aminoacetic acid chelating agent has a low water solubility, and the nitrogen triacetic acid has the paper size applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm). I 11 11 I order ~ I-1 , 1111 - (Please read the notes on the back and fill in the 3 pages) - Refill JR* / Ministry of Economic Affairs Intellectual Property Bureau Staff Consumer Cooperatives Print A7 1278480 B7___ V. Description of invention (5) High solubility in water. Thus, the inventors of the present invention have completed the present invention, and have found that an aminoacetic acid chelating agent has a total reduction in the total content of nitrogen triacetic acid (salt) in the water-absorbent resin, which is determined by utilizing the difference in water solubility described above. The method comprises the steps of: adjusting the p Η値 of the aqueous solution of the aminoacetic acid chelating agent containing nitrogen triacetic acid (salt) therein to a range of 1 to 3 to deposit a precipitate (acid form of the aminoacetic acid chelating agent) The deposited precipitate is recovered via its separation; and if necessary, rinsed and then dried to recover the precipitate. Thus, in order to solve the above problems, the present invention provides the following items: (1) A water-absorbent resin composition comprising a water-absorbent resin and an aminoacetic acid chelating agent, wherein the aminoacetic acid chelating agent in the water-absorbent resin composition The mixing ratio is not less than 10 ppm of the water-absorbent resin, and the total content of the nitrogen triacetic acid and the salt thereof in the water-absorbent resin composition is not more than 1 ppm of the water-absorbent resin composition. (2) A water-absorbent resin composition comprising a water-absorbent resin and an aminoacetic acid chelating agent, wherein the total content of the nitrogen triacetic acid and the salt thereof is not more than 1 in respect to the aminoacetic acid chelating agent in the water-absorbent resin composition. 0 0 0 ρ pm 〇 (3) The water-absorbent resin composition according to (1) or (2) above, which further comprises a water-soluble deodorant. (4) The water-absorbent resin composition according to any one of the above (1) to (3), which exhibits an absorption capacity under no load of not less than 30 g/g, and a deteriorated extractable content of the elution Not more than 20% by weight, the absorption capacity under the load of 1. 9kPa is not less than 28g/g, and the paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) (please read the back first) Note on this page)
Printed by the Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumer Cooperatives &amp; 1278480 A7 . _B7 __ V. Invention Description (6) The yellow index is not higher than 26. (5) A water-absorbent resin composition comprising a water-absorbent resin and a water-soluble deodorant and exhibiting an absorption capacity under no load of not less than 30 g/g, and the amount of deteriorated extractables of the elution is small At 20% by weight, the absorption capacity under the load of 1 · 9 k P a is not less than 28 g / g ' and the proportion of the odor of vomiting is not less than 40%. These and other objects and advantages of the present invention will be more fully apparent from the Detailed Description. BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 illustrates a measurement device for the absorption capacity under load. Main component comparison (please read the note on the back and fill in the 3 pages): Fill the Ministry of Economic Affairs, Intellectual Property Bureau, Staff Consumer Cooperative, Print 1. Scale 2 Container 2a Opening 2b Opening 3 Intake Pipe 3a Bottom 4 Conduit 5 Measuring Part 6 Glass Filter 7 Paper filter 9 Support cylinder set V—-----line
This paper scale is applicable to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Β7 V. Invention description (7) 10 Metal mesh 11 Weight 12 Water-soluble sodium chloride solution 13 Water-absorbent resin (composition) 15 Water-absorbent resin (composition) Detailed Description of the Invention The water-absorbent resin composition according to the present invention comprises a water-absorbent resin and an aminoacetic acid chelating agent, wherein a mixture ratio of the aminoacetic acid chelating agent in the water-absorbent resin composition is quite large The water-absorbent resin is 1 〇 ppm, and the total content of the nitrogen triacetic acid (salt) in the water-absorbent resin composition is not more than 1 ppm of the water-absorbent resin composition. This limitation can be easily achieved, for example, in a method in which an aminoacetic acid chelating agent is used as an aminoacetic acid chelating agent, and the total content of nitrogen triacetic acid (salt) in the aminoacetic acid chelating agent is not more than 1, 〇〇 〇ppm aminoacetic acid chelating agent. However, it is not limited to this method. The aminoacetic acid chelating agent having the total low nitrogen triacetic acid (salt) content is not limited, but can be obtained, for example, from a method comprising the steps of adjusting the p Η値 range of an aqueous solution of a commercially available aminoacetic acid chelating agent. At 1 to 3, to deposit a precipitate in which the aminoacetic acid chelating agent contains nitrogen triacetic acid (salt) as an impurity; and then, by separating therefrom, the deposited precipitate is recovered, and the amino group containing nitrogen triacetic acid (salt) therein is contained therein. The method of adjusting the 水溶液 of the acetic acid chelating agent Ρ 无 in the range of 1 to 3 is not particularly limited. The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) (please read the notes on the back first) Re-filling page) Re-subscribing----^----- Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing B7___ five, invention description (8) but Execution may be carried out by adding an acid such as sulfuric acid, nitric acid, or hydrochloric acid to the above aqueous solution. The pH of the aqueous solution is preferably adjusted so as to range from 1.5 to 2.5, and more preferably from 1 to 8 to 2.0. This is simply performed by filtration to recover the precipitate. The precipitate recovered by the separation is preferably washed with pure water, and the dried precipitate is preferably dried at a temperature of from 50 to 200 °C. By the above method, the total content of the nitrogen triacetic acid (salt) in the aminoacetic acid chelating agent can be reduced to not more than 1,000 ppm, preferably not more than 500 ppm, more preferably not more than 200 ppm, and more preferably Not more than 100 p pm of aminoacetic acid chelating agent. If the aminoacetic acid chelating agent obtained from the above method having an extremely reduced total content of nitrogen triacetic acid (salt) is added to the water absorbent resin or its raw material, the nitrogen triacetic acid in the water absorbent resin composition The total content of (salt) may become very low, in particular, preferably not more than 1 ppm, more preferably not more than 0.5 ppm, and more preferably no more than 〇·lppm, and even more preferably not More than this water-absorbent resin composition 〇. 〇1 p pm. When the aminoacetic acid chelating agent is added to the water-absorbent resin or its raw material, there is no particular limitation, but, for example, an aminoacetic acid chelating agent may be added to the (1) monomer, or (2) the resulting gel, or during polymerization or After the polymerization, or (3) during the surface crosslinking treatment, or (4) after the surface crosslinking treatment, or (5) in the recovery step of recovering the water-absorbent resin fine particles. It is especially preferred to add during or after the surface crosslinking treatment. The aminoacetic acid chelating agent may be added to the water absorbent resin or its raw material, and dissolved or dispersed in water or an organic solvent (for example, methanol, ethanol, isopropanol *44-=_ (please read the back of the note first) · K-- "Filling" Order r---------- line
This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing __ _B7 _ five, invention description (9), acetone), but better It is preferred that the latter be added after the dissolution of the alkali solution. [Because, as described above, this acid form has a low water solubility. The concentration of the aminoacetic acid chelating agent solution is preferably from 0.1 to 40% by weight, more preferably from 1 to 40% by weight. The aminoacetic acid chelating agent may be added to a water-absorbent resin having a content ranging from 1 P pm to 10% by weight, preferably from 5 to 1,000 ppm, more preferably from 10 to 800 p pm. When the amount of the aminoacetic acid chelating agent used is too small, the urine resistance promoting effect will not be seen. When the amount of the aminoacetic acid chelating agent used therein is too large, a satisfactory effect of this amount cannot be obtained. In the resulting water-absorbent resin composition, the amount of the aminoacetic acid chelating agent relative to the water-absorbent resin depends on how the aminoacetic acid chelating agent is added to the water-absorbent resin, but is substantially the same as the above-mentioned addition of the water-absorbent resin. The amount of glycine chelating agent. Examples of the aminoacetic acid chelating agent which can be used include ethylenediaminetetraacetic acid, hydroxyethylethylidenediaminetriacetic acid, diethylidenetriaminepentaacetic acid, tris-ethyltetraaminehexaacetic acid, and cyclohexane. Aminotetraacetic acid, and its basic metal salts, surface salts, and amine salts, particularly preferably di-ethyltriamine pentaacetic acid, tri-ethylidenetetraamine hexaacetic acid, and alkali metal salts thereof class. A water-absorbent resin which can be used for the water-absorbent resin composition according to the present invention, which can absorb a large amount of water in water to form a water gel, and examples thereof include those having a carboxyl group, in particular, for example, partial neutralization. And cross-linked poly(acrylic acid): hydrolyzed starch-acrylonitrile graft polymer; neutralized starch-acrylic graft polymer; saponified vinyl acetate-propion; please read the back note Fill in: Fill in this page) Order·,——一-----Line/ This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 42 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative制备一—___B7____ V. DESCRIPTION OF THE INVENTION (10) Copolymer of a enoate; crosslinked carboxymethylcellulose polymer; hydrolyzed copolymer of acrylonitrile or acrylamide or a hydrolyzed copolymer Crosslinked polymer; crosslinked polymer of cationic monomer; crosslinked isobutylene-maleic acid copolymer; and crosslinked 2-propionylamino-2-methylpropane sulfonate A copolymer of acid-acrylic acid. The most preferred of these is a partially neutralized and crosslinked poly(acrylic acid). This partially neutralized and crosslinked poly(acrylic acid) can be obtained from a process which includes the step of polymerizing a hydrophilic monomer, and this single The body includes a major proportion of acrylic acid and/or a salt thereof. The proportion of the monomer other than the acrylic acid and/or its salt is preferably not more than 3 〇m ο 1 % of the monomer component. For this neutralization ratio, it is preferred that the acid group is neutralized at 50 to 95 mol%, more preferably 60 to 90 m〇1%. Examples of such salts include basic metal salts, ammonium salts, and amine salts. It is preferred to carry out aqueous solution polymerization or reverse phase suspension polymerization as a polymerization method. For cross-linking a partially neutralized poly(acrylic acid) derived from this polymerization, a self-crosslinking type of locally neutralized poly(acrylic acid) which does not require a crosslinking agent may be used, but this locally neutralized polycondensation is preferred. (Acrylic acid) is copolymerized or reacted with an internal crosslinking agent having at least two polymerizable unsaturated groups or at least two reactive groups per molecule. Specific examples of the internal crosslinking agent include: hydrazine, Ν'-methylenebis(meth) acrylamide, (poly)ethylene glycol di(meth) acrylate, (poly)propylene glycol di(methyl) Acrylate, trimethylolpropane tri(meth)acrylate, tris(meth)acrylate, glycerol acrylate methyl acrylate, ethyl epoxide-modified dimethylolpropane three (4^ _ (Please read the notes on the back and fill in the I^ page) Order-----------
This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) A7 1278480 __B7 V. Description of invention (n) Methyl) acrylate, pentaerythritol tetra(meth) acrylate, diisoprene Tetraol hexa(meth) acrylate, triallyl cyanurate, triallyl isocyanurate, triallyl phosphate, triallylamine, poly(methyl) ene Propoxyalkyl, (poly)ethylene glycol diglyceryl ether, glyceryl diglyceryl ether, ethylene glycol, polyethylene glycol, propylene glycol, glycerin, isovaerythritol, ethylene diamine, vinyl acid salt, propylene Carbonate, polyethyleneimine, and glyceryl (meth) acrylate. Such internal crosslinking agents can be used singly or in combination with each other. The amount of the internal crosslinking agent to be used is preferably in the range of from 0. 005 to 3 mol, more preferably from 〇1 to 1.5 m. Too small amounts of internal crosslinkers tend to result in low liquid permeability and absorption rate. On the other hand, too much internal crosslinking agent tends to cause low absorption capacity. Printed by the Intellectual Property Office of the Ministry of Economic Affairs, the Consumer Cooperatives. When the polymer produced from the above polymerization is a water gel, the water gel is required to be finely divided into a predetermined particle size in order to dry the water gel afterwards. Fine particle formation of the water gel, which can be carried out, for example, by polymerization using a double-arm kneader during polymerization, or by performing extrusion from a die of, for example, a chopper. In addition, the fine particle formation can also be carried out using, for example, a cutting mill. The particle size of the finely divided gel may suitably be set according to the ability of the dryer, but generally preferably ranges from 0. 1 to 10 mm. When the granulated gel is finer than 〇 1 mm, the resulting water-absorbent resin may have poor physical properties. When the granulated gel is coarser than 1 〇 m m, the gel may be difficult to dry. In this fine particle formation step, a coarse _---14 particle size greater than 1 〇mm can be formed. The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm). A7 1278480 ___ B7 V. Description of the invention (12) Gel and fine gel with a particle size of less than 0.1 mm. Such polymers can be separated and then added, for example, in a water soluble monomer solution or in a polymer gel. The finely divided gel in the above fine particle formation step is dried in the drying step. Examples of the drying device which can be used include a hot air dryer, a gas flow dryer, a fluidized bed dryer, a drum dryer, a microwave oven, and a far infrared furnace. The drying temperature is usually not lower than 120 ° C, preferably in the range of from 1 50 to 250 ° C, more preferably in the range of from 1 60 to 220 t:. The resulting dried product is honed (if necessary) and then classified by a sieve having a predetermined size, and as a result, a water-absorbent resin powder having an average particle diameter of from about 10 to about 1,000 / zm, preferably, is obtained. From about 1 〇〇 to about 700 / / m, more preferably from about 300 to about 50 0 / m, and wherein the proportion of fine particles less than 168 is not more than 5% by weight, preferably not much It is 3% by weight, more preferably not more than 1% by weight. The fine particles of the water-absorbent resin removed by classification can be recycled and then used, and then added to any step of preparing the water-absorbent resin. The Ministry of Economic Affairs, the Intellectual Property Office, the employee consumption cooperative, prints the recycled water-absorbent resin (subtle The particle diameter of the particles is not particularly limited, but is generally not more than 300/zm, preferably not more than 2 2 5 / / m, and more preferably not more than 15 0 / / m. The recovered water-absorbent resin may be after the surface cross-linking treatment or the surface cross-linking treatment, and both water-absorbent resinizations may be used. In order to recycle the recovered fine particles, water is added thereto to make them granulate. The amount of water to be added is preferably in the range of 0.1 to 2,000 parts by weight, more preferably 10 to 900 parts by weight, per one of the paper sizes applicable to the Chinese National Standard (CNS) A4 specification (210 X 297). 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printed B7__ five, invention description (13) 100 parts by weight of water-absorbent resin meter. When the amount of water added therein is less than the above range, it will be difficult to reuse it. Further, when the amount of water added therein is larger than the above range, the reused water-absorbent resin is liable to be deteriorated. When an aminoacetic acid chelating agent is added in the step of reusing the fine particles, an aqueous solution of a chelating agent may be added to the fine particles, or a chelating agent may be added to a mixture of water and the fine particles. In addition, it is also permissible to mix the chelating agent with a dry blend of fine particles with water. Cross-linking treatment in the vicinity of the surface of the water-absorbent resin powder can further improve the water absorbing property, in particular, the absorption capacity of the absorbent resin under water under load. Examples of such surface crosslinking agents include those disclosed in JP-A-180233/1983, JP-A-016903/1986, JP-A189103/1984, JP-A-117393/1977, JP-A-136588/1976, JP-A-257235/1986, JP-A-007745/1987, JP-A-211305/1986, JP-A-252212/1986, JP-A-264006/1986, German Patent No. 4020780, W〇99/ 42494, WO 99/43720, W〇00/31153, and JP-A 197818/2000. In particular, it is not limited to the surface crosslinking agent, if it has at least two functional groups which are reactive with the surface functional groups of the water-absorbent resin. Examples of the surface crosslinking agent include: polyol compounds such as ethylene glycol, diethylene glycol, propylene glycol, triethylene glycol, tetraethylene glycol, poly (please read the back sheet of the precautions and fill in the page): -*-----line
V This paper size applies to China National Standard (CNS) A4 specification (210 X 297 mm) A7 1278480 B7__ V. Description of invention (14) Ethylene glycol, 1,3 -propanediol, dipropylene glycol, 2,2,4 Trimethyl-1,3-1,3-pentanediol, polypropylene glycol, glycerin, polyglycerol, glycerophosphoric acid, 2-butene-1,4-diol, 1,3-butanediol, 1,4 butyl Glycol, 1,5-pentanediol, 1,6-hexanediol, 1,2-cyclohexanedimethanol, 1,2-cyclohexanol, trimethylolpropane, diethanolamine, triethanolamine, Polyoxypropylene, oxyethylene-oxypropylene block copolymer, pentaerythritol and sorbitol; polyepoxy compounds such as ethylene glycol diglyceryl ether, polyethylene glycol diglyceryl ether, glycerol polyglyceryl Ether, diglycerin polyglyceryl ether, polyglycerol polyglyceryl ether, propylene glycol diglyceryl ether, polypropylene glycol diglyceryl ether and deglycerin; polyamine compounds such as ethylenediamine, diethylenediamine, three Ethyltetramine, tetraethylidene pentaamine, pentaethylhexamine and polyethyleneimine, and inorganic or organic salts thereof (eg 'nitrogen tetramine a polyisocyanate compound such as 2,4-tolyl diisocyanate and hexamethylene diisocyanate; a polydihydrocarbazole compound such as 1' 2 -ethylidenedi-dihydroterboxazole, polyisopropenyldihydrogen Azone, and copolymers thereof; alkyl carbonate compounds such as 1,3 -dioxol-2-one, 4-methyl-1,3-dioxol-2-one, 4,5-Dimethyl-1,3-dioxol-2-one, 4,4-dimethyl-1,3-dioxol-2-one, 4-ethyl a 1, 3-dioxol-2-one, 4-hydroxymethyl-1,3-dioxol-2-one, 1,3-dioctane-2-one, 4 —Methyl—1,3—dioctane-2-one, 4,6-dimethyl-1,3-dioxane-2-one and 1,3-diketopentan-2-one; halogen Epoxy compounds such as epichlorohydrin, epibromohydrin and alpha-methylepichlorohydrin, and their poly-17 - paper scales are applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) &lt; Read the precautions on the back and fill in the form: Fill in the page
Ministry of Economic Affairs Intellectual Property Office Staff Consumer Cooperatives Printed A7 1278480 __B7___ V. Invention Description (15) Month female adduct (eg 'Kymene (registered trademark), produced by Hercules); decane coupling agent such as 7-glycidoxypropyl And triethyl methoxy decane; and polyamino metal compounds such as the following hydroxides and chlorides: zinc, calcium, magnesium, aluminum, iron and chromium. Among them, preferred are polyhydric alcohol compounds, polyepoxy compounds, polyamine compounds or salts thereof, and alkylene carbonate compounds. Such surface crosslinking agents can be used singly or in combination with each other. The amount of the surface crosslinking agent, when used, is preferably in the range of from 0.01 to 10 parts by weight, more preferably from 0.1 to 5 parts by weight, per 100 parts by weight of the water-absorbent resin. . When the amount of the surface crosslinking agent to be added is less than 0.1 part by weight, the surface crosslinking will be insufficient. When the amount of the surface crosslinking agent is more than 10 parts by weight, the resulting absorption capacity may be extremely low. Printed by the Intellectual Property Office of the Intellectual Property Office of the Ministry of Economic Affairs, after mixing the water-absorbent resin with the surface crosslinking agent, the resulting mixture may be heat treated if necessary. A conventional dryer or furnace can be used for the heat treatment, and examples thereof include a tunnel type agitating dryer, a rotary dryer, a disk dryer, a fluidized bed dryer, a gas flow dryer, and an infrared dryer. When the heat treatment is performed, the heat treatment temperature is preferably in the range of 40 to 250 ° C, more preferably 90 to 230 ° C, and still more preferably 1 2 0 to 2 2 ° ° C. When the heat treatment temperature is lower than 40 ° C, heat treatment is required for a long time to lower the productivity. On the other hand, when the heat treatment temperature is higher than 250 ° C, there is a danger that the water absorbent resin may be thermally deteriorated due to the use of a water absorbent resin. The heating process usually has a preferred range of 1 to 120 minutes, and more _:_ia -_ This paper scale applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm). 1278480 A7 Ministry of Economic Affairs Intellectual Property Office staff consumption Cooperatives printed B7 V. Inventions (16) The best is between 10 and 60 minutes. When an aminoacetic acid chelating agent is added in the surface crosslinking treatment step, the water-absorbent resin is mixed with a surface crosslinking agent and an aminoacetic acid chelating agent, and if necessary, the resulting mixture is subjected to heat treatment. In the above mixing step, it is preferred to use water. The water amount is preferably in the range of from 0.5 to 10 parts by weight, more preferably from 0.5 to 3 parts by weight per 100 parts by weight of the water-absorbent resin. When the amount of water added therein is less than the above range, it will be difficult to fix the aminoacetic acid chelating agent to the surface of the water absorbent particles. Further, when the amount of water added therein is larger than the above range, the absorption capacity of the water absorbent resin may be lowered. The conditions of the heat treatment are the same as those in which the aminoacetic acid chelating agent is not added. When the aminoacetic acid chelating agent is added after the surface crosslinking treatment step, it is preferred to add the amino acid, the chelating agent and water to the water-repellent resin which has been subjected to cross-linking treatment by spraying, thereby bonding the particles of the water-absorbent resin to each other. Water is used as a binder, so that it is granulated. Thereby, the aminoacetic acid chelating agent can be immobilized on the surface of the upper water absorbent resin. Since the deterioration of the water-absorbent resin due to urine occurs on the surface of the resin, the urine resistance can be enhanced by placing the aminoacetic acid chelating agent in the vicinity of the surface of the water-absorbent resin. The preferred range of the amount of water used herein is from 0.1 to 20 parts by weight, more preferably from 0.1 to 10 parts by weight, and even more preferably from 0.5 to 4 parts by weight per 1 part. 0 parts by weight of the water-absorbent resin. When the amount of water to be added is less than the above range, it will be difficult to granulate the water absorbent fine particles' and further, it will be difficult to fix the aminoacetic acid chelating agent to the surface of the water absorbent fine particles. In addition, when the amount of water added is larger than the above range, water absorption (please read the notes on the back and fill in the page)
:fill? R order.·---.-----line
V This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing __Β7 5, invention description (17) resin swelling and reaching the inner part The gel is formed, so that the particulate product in the target may not be obtained, and further the surface crosslinked layer on the surface of the water absorbent particle may be broken. The water-absorbent resin composition according to the present invention may further comprise a water-soluble deodorant to exhibit deodorizing properties of the water-absorbent resin composition. Incidentally, the reason why the water-soluble one is used as the deodorant is that the water-soluble deodorant can impart excellent deodorizing property to the water-absorbent resin composition without deteriorating the absorption property of the water-absorbent resin composition. Here, the water-soluble deodorant is used in an amount of not less than 0 lg, preferably not less than lg, more preferably not less than 10 g of a deodorant, and is soluble in 100 g of deionized water in the room. Warm down. For the deodorant, various conventionally extracted essential oils such as those extracted from the leaves of Camellia can be used. Examples of Camellia plants include camellia, tea tree, Christmas camellia, sakaki plant, and scarlet sakah plant, and deodorizable ingredients extractable from the leaves using an organic solvent. Such as alcohols and ketones, or water, or a mixture of solvents. This extraction component includes flavanols, flavanols, organic polymers, or tannins. The mixing ratio of the deodorant is preferably in the range of 〇 〇 〇 〇 1% by weight (1 p pm) to 10% by weight of the water-absorbent resin. When the mixing ratio of the deodorant is less than the above range, the deodorizing effect will not be exhibited. Further, when the mixing ratio of the deodorant is larger than the above range, the effect of increasing the cost is not obtained. The deodorant is mixed into the water-absorbent resin composition, and the deodorant may be dissolved into water or an organic solvent such as an alcohol, for example, by 1), and then the resulting solution is sprayed onto the water-absorbent resin (or a composition thereof): or 2) Add the deodorant to the solvent along with the water-absorbent resin (please read the precautions on the back and fill in the JR page).···.-----Line
V The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) 2α A7 1278480 -- _B7__ 5. Inventive Note (18), and the solvent does not swell the water-absorbent resin (or its composition) And then co-stirring together to form a mixture, and then removing the solvent from the mixture; or 3) powdering or granulating the deodorant, and then mixing the resulting powder or granules with a water-absorbent resin (or Its composition). Preferably, a deodorant is added simultaneously to the above granulation or addition of a chelating agent. Examples of the deodorant other than the above-mentioned extracted essential oil extracted from the leaves of the Camellia plant include: organic acids such as acetic acid, citric acid, and lactic acid; sodium chloroausole; copper chloroausin; cyclodextrin; and flavonoids Compound. The mixing ratio of such other deodorant is preferably in the range of from about 0. 0.001 wt% (1 p pm) to about 10 wt% of the water-absorbent resin. The above-mentioned water-absorbent resin composition according to the present invention has the following properties: · Printed by the Ministry of Economic Affairs, Intellectual Property Office, and the Consumer Cooperatives (1) The absorption capacity under no load is not less than 30 g/g, preferably Not less than 34 g/g, more preferably not less than 40 g/g; the deteriorated extractables content of the dissolution is not more than 20% by weight, preferably not more than 18% by weight, more preferably not more than 16 % by weight; the absorption capacity under a load of 1.9 kPa is not less than 28 g/g, preferably not less than 30 g/g, more preferably not less than 32 g/g; and the yellowness index is not more than 26 Preferably, no more than 24, and more preferably no more than 22. (2) The absorption capacity under no load is not less than 30 g/g, preferably not less than 34 g/g, more preferably not less than 40 g/g, and the content of degraded extractables in the dissolution is not More than 20% by weight, preferably not more than 18% by weight, 5 more preferably not more than 16% by weight; the absorption capacity under a load of 1 · 9 kPA is not less than 28 g/g, preferably Not less than -______ This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing 1278480 a7 ____B7 _ V. Invention description (19) 30g/g, more The best is not less than 32g / g; and the proportion of the scent reduction is not less than 40% 'better than not less than 45 % 'better than not less than 50% ° when one is in no A water-absorbent resin composition exhibiting an absorption capacity of less than 30 g/g under load is used for the absorbent article. This absorbent article has a small absorption amount and will easily leak. When the water-absorbent resin composition 'for the absorbent article' having a deteriorated extractable content of more than 20% by weight exhibiting dissolution is given for a long time, it gives a disgusting feeling. When the water-absorbent resin composition exhibiting an absorption capacity of less than 2 8 g / g under a load of 1.9 kPa is used for the absorbent article, the absorption amount of the absorbent article is small and its leakage easily occurs. When a water-absorbent resin composition exhibiting a yellowness index of more than 26 is used for an absorbent article such as a disposable diaper and a sanitary napkin, the absorbent article will be easily discolored during storage, and the absorbent resin will be used. The composition can be seen through the surface of the absorbent article. If the yellowing index is not more than 2 6, the storage durability will be good, and further, the water-absorbent resin composition cannot be seen through the surface of the absorbent article, and as a result, the customer complains lower. When a water-absorbent resin composition exhibiting a disgusting odor reduction ratio of less than 40% is used for a diaper, the deodorizing effect is low or not fully exhibited. However, if a water-absorbent resin composition exhibiting a disgusting odor reduction ratio of not less than 40% is used, a deodorizing effect can be seen. With respect to the water-absorbent resin composition according to the present invention, the water-absorbent resin composition can be allowed to obtain a new function, and the Chinese National Standard (CNS) A4 specification (210 X 297 mm) is applied by adding some of the materials such as the fragrant paper. Please read the notes on the back first.
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22 A7 1278480 B7 _ V. INSTRUCTIONS (20) Materials, chemicals, plant growth adjuvants, fungicides, foaming agents, pigments, dyes, and fertilizers. The water-absorbent resin composition according to the present invention comprises various shapes such as irregular particles, pulverized shape, spherical shape, strip shape, and granular shape, and has a weight average particle diameter preferably in a range 1 〇〇 to 600//ΓΠ, and better at 200 to 500/zm. Further, the proportion of the water absorbent resin in the water absorbent resin composition is usually not less than 75 wt%, preferably not less than 85 wt%, more preferably not less than 95 wt% of the water absorbent resin composition. . Printed by the Intellectual Property Office of the Ministry of Economic Affairs, the Consumers' Cooperatives, the water-absorbent resin composition according to the present invention not only absorbs water, but also absorbs various liquids such as body fluids, physiological saline solution, urine, blood, cement water, and fertilizers. Water, and which may advantageously be used not only in sanitary materials such as disposable diapers, sanitary napkins and incontinence pads, but also in various industrial fields such as engineering work, agriculture and horticulture, but particularly advantageously Sanitary materials, such as disposable diapers (including baby defecation training pants with disposable diapers) and incontinence pads, which utilize excellent urine resistance using a water-absorbent resin composition. The sanitary material is used for the purpose of absorbing urine. Next, the absorbent article will be described here, and the absorbent article is a water-absorbent resin composition according to the present invention. An absorbent article comprising the water-absorbent resin composition according to the present invention, comprising: an absorbent layer comprising a material of the water-absorbent resin composition of the present invention and a fiber; a liquid permeable surface sheet; and a liquid impervious The backing plate; wherein the water-absorbent resin composition is applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) for the water-absorbent resin composition and the paper size of the fiber 22^ A7 1278480 ----_B7___ V. Description of the invention (21) The weight ratio of the total amount of the material, α, usually not less than 〇. The weight ratio α preferably ranges from 0.3 to 1.0, and more preferably from 0.4 to 0.8. When the above weight ratio α is less than 〇. 2, the resulting absorbent article is generally bulky and exhibits too high desorption (wet back). In particular, the water-absorbent resin composition of the present invention is very preferred because the resin composition becomes very little discolored, evolves over time in the initial stage and after production, and thus has no problem of discoloration, even if The water-absorbent resin composition makes α not less than 〇·2 at a high concentration. Further, if the water-absorbent resin composition according to the present invention which satisfies the above definition of the disgusting odor reduction ratio is used in a high concentration, and α is not less than 0.2, the deodorizing effect will be very preferably high. . Ministry of Economic Affairs, Intellectual Property Office, Staff Consumer Cooperative, printed in the method of preparing the absorbent article, the water absorbent resin composition is blended or sandwiched into the fiber material to prepare an absorbent structure (absorbent core), and will be generated The absorbent core is sandwiched between a liquid permeable surface material and a liquid impermeable substrate material, and the resulting product, if desired, is provided with a variety of materials such as elastic members, diffusion layers, or pressure sensitive Adhesive tape, thus obtaining absorbent articles, in particular, sanitary napkins or adult diapers. The above absorbent core is compression-molded so as to have a density of from 0.06 to 0.5 g/cc and a basis weight of from 〇·〇1 to 〇.20 g/cm2. Incidentally, examples of the fiber material that can be used include hydrophilic fibers such as honed wood pulp, and other examples include cotton linters, crosslinked cellulose fibers, crepe, cotton, wool, acetate, and Vinon (vinyl on). Preferably, he can be used for air laying. This paper scale applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm). 24 A7 1278480 _____Β7____ V. Inventive Note (22) (Effects and Advantages of the Invention): The water-absorbent resin composition according to the present invention contains an amino group Acetic acid chelating agent, and the total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition is very low, so the water-absorbent resin composition has excellent urine resistance and further excellent light resistance and change Very little discoloration and high safety. When the water-absorbent resin composition further contains a water-soluble deodorant, it also solves the problem that occurs when the water-absorbent resin absorbs urine, for example. The water-absorbent resin composition according to the present invention further exhibits excellent absorption capacity under no load, excellent degraded deteriorated extractables content, and excellent absorption capacity under load. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT OF THE INVENTION Hereinafter, the present invention will be more specifically described by way of the following examples of preferred embodiments of the present invention as compared with the comparative examples not according to the present invention. However, the invention is not limited thereto. Printed by the Intellectual Property Office of the Ministry of Economic Affairs, the Consumer Cooperatives, unless otherwise stated, the unit "parts" and "%" and the term "water-absorbent resin (composition)", as briefly mentioned below, represent "parts by weight" respectively. , "% by weight", and "water-absorbent resin or water-absorbent resin composition". (1) Absorption capacity of water-absorbent resin (composition) under no load First, 0. 2 g of water-absorbent resin (composition) was uniformly placed in a tea bag type packet (6 cm X 6 cm). Then, the opening is sealed by heating, and then the bag is immersed in a 0. 9 % water-soluble paper at room temperature. The Chinese National Standard (CNS) A4 specification (210 X 297 mm) 2^, A7 1278480 B7__ DESCRIPTION OF THE INVENTION (23) Sodium chloride solution (physiological saline). After 60 minutes 'and then under 50 g (cm / sec 2 ), the packet was taken out by centrifugation to discharge the liquid for 3 minutes, and then measured The weight of the packet W i (g). On the other hand, the same step ' is performed using the non-absorbent resin (composition) and the generated weight W 〇 (g) is measured. Thus, the weight is calculated according to the following formula at no load. Absorption capacity below (g/g): Absorption capacity under no load (g/g) = (W^-Wo) / (weight of water-absorbent resin (composition) (g)) (2) The extractable material eluted from the self-water-absorbent resin (composition) contains halo. First, 2 5 in a 100 ml beaker. 1 g of the water-absorbent resin (composition) was swollen in the liter of artificial urine, and the beaker was sealed and then allowed to stand at 37 ° C for 16 hours. Then, the resulting swelling gel was dispersed into 9 7 5 In milliliters of deionized water, the eluted extractables were rinsed with deionized water, dispersed and stirred for 1 hour and then filtered through a paper filter. Then '50 g of this filtrate was placed in 100 mL. In a beaker, add 1 ml of 0 · 1 N water-soluble sodium hydroxide solution, 10 ml of N/2 0 water-soluble methyl glycol polyacetamide chitin solution, and 4 drops of 〇·1 % water-soluble toluidine blue solution, and then the solution formed in the above beaker is titrated with N/40 0 water-soluble poly(potassium vinyl sulfate) solution, when the color of the solution changes from blue to light' The reddish purple point is regarded as the end point of the titration to determine the titer B i (ml). In addition, the same procedure can be performed for the non-absorbent resin (composition) to determine the titer (: 1 (ml) as a blank. Then According to the following formula, the paper scale applies to the Chinese National Standard (CNS). A4 size (210 X 297 mm) (Please read the notes on the back and then fill in this page) Order I--------- Line
Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumer Cooperatives, Printing A7 1278480 __B7__ V. Description of Invention (24) The titer B: and (:i and the molecular weight D i of the repeating unit of the water-absorbent resin) can be calculated from the self-absorbent resin. (Composition) Extractable extractables content (wt%): Analyzable extractables content (wt%) ^(Ci-BnxO.OOSxDi. The composition of this artificial urine is as follows:
Deionized water 9 7 · 1 % Urea 1.9% Sodium chloride 0.8% Magnesium chloride 0.1% Calcium chloride 0.1% (3) Degradable extractable content of self-absorbent resin (composition)
Printed by the Ministry of Economic Affairs, the Intellectual Property Office, and the Consumer Cooperatives. First, in the 100 ml plastic container with a lid, 1 g of the water-absorbent resin (composition) is swollen to 25 times with artificial urine. The liquid contained L-ascorbic acid at a concentration of wt·〇〇 5 wt%, and the container was closed and then allowed to stand at 37 ° C for 16 hours. Thereafter, the resulting swelling gel was dispersed in 975 g of deionized water to rinse the precipitated deteriorated extractable component with deionized water. This dispersion was stirred for 1 hour and then filtered through a paper filter. Next, 50 g of the resulting filtrate was placed in a 100 ml beaker. Add 1 ml of 0.1N water-soluble sodium hydroxide solution, 10 ml of N / 200 water-soluble methyl glycol polyacetamide chitin solution, and 4 drops of 0.1% water-soluble toluidine blue solution. And then use the N/40 0 water private paper scale for the solution generated in the above beaker to apply the Chinese National Standard (CNS) A4 specification (210 X 297 mm) - 2Z - 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative _ B7___ _ V, invention description (25) soluble poly (potassium vinyl sulfate) solution for colloidal titration, when the color of the solution changes from blue to reddish purple as the end point of the titration to determine the titer B 2 ( ML). Further, the same procedure was carried out without using a water-absorbent resin (composition) to determine a titer C 2 (ml) as a blank. Then, the content of the deteriorated extractables (wt%) eluted from the water-absorbent resin (composition) was calculated from such titers B 2 and (2) and the molecular weight D 2 of the water-absorbent resin repeating unit according to the following formula. : Degradation of extractables content (wt % ) = (C2 - 132) x 0.005 x D2 〇 (4) Absorption capacity under load: The absorption capacity under load is measured using the measuring device of Figure 1. In Fig. 1, the measuring device comprises: a scale 1; a container 2 mounted on the scale 1 with a predetermined capacity; an intake pipe 3; a conduit 4; a glass filter 6; and, if mounted on the glass filter 6, Measuring section 5. The container 2 has an opening 2 a on the top and an opening 2 b on the side. The intake pipe 3 is inserted through the opening 2 a and the duct 4 is mounted on the opening 2 b. Further, the container 2 is preliminarily mounted Determine the amount of 0. 9 % water-soluble sodium chloride solution (hereinafter referred to as physiological saline solution) 1 2. The lower part of the intake pipe 3 is immersed in the physiological saline solution 1 2 . Set the intake pipe 3 to make the internal pressure of the container 2 It is kept at substantially atmospheric pressure. The diameter of the glass filter 6 is 55 mm. The container 2 and the glass filter 6 are via The conduits 4 made of ketone resin are connected to each other. Further, the position and height of the glass filter 6 are fixed relative to the container 2. The measuring portion 5 comprises: a paper filter 7; a support cylinder 9; as attached to the bottom of the support cylinder 9 The metal mesh 1 0 ; and the weight 1 1 . The formation of the measuring part 5 - 2S - Please read the note on the back first
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Good paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) A7 1278480 B7 V. Inventive Note (26) Insert the paper filter 7 and the support cylinder 9 (ie metal mesh 1 依) in sequence On the glass filter 6. The metal mesh 10 is made of stainless steel and has a mesh opening size of 400 mesh (38/m). The height of the metal mesh, in other words, the height of the contact surface of the metal mesh 10 and the water absorbent resin (composition) 15 is set to be the same height as the bottom surface 3a of the 进气f intake pipe 3. On the metal mesh 10, a predetermined amount of the water-absorbent resin (composition) 15 is uniformly spread. The weight of the weight 11 is adjusted so that the load can be uniformly applied to the metal mesh 1 4 at 4·83 kPa or 1.9 kPa, in other words, to the water absorbent resin (composition) 15 . A measuring device having the above composition was used to measure the absorption capacity under load. The measurement method is explained below. Printing by the Intellectual Property Office of the Ministry of Economic Affairs, the Consumers' Cooperatives First, a predetermined preparatory operation is carried out in which, for example, a predetermined amount of physiological saline solution 12 is placed in the container 2, and the intake pipe 3 is inserted into the container 2. Next, the paper filter 7 is mounted on the glass filter 6. On the other hand, parallel to such a mounting operation, 0·9 g of the water-absorbent resin (composition) 15 is uniformly distributed inside the support cylinder 9, in other words, on the metal mesh 10, and the weight is 1 1 is placed on the water-absorbent resin (composition) 15. Next, the metal mesh 10, in other words, the support cylinder 9 (in which the water absorbent resin (composition) 15 and the placed weight 1 1 ) ' is mounted on the paper filter 7 so that the center line of the support cylinder 9 will It conforms to the center line of the glass filter 6. Then, the weight of the physiological saline solution absorbed by the water-absorbent resin (composition) 15 in the period from 60 minutes after the support cylinder 9 was mounted on the paper filter 7 was measured by the scale 1. In addition, 'the same procedure as above is performed without using the water-absorbent resin (composition) 15 '. The scale of the paper is measured by the scale 1 and the Chinese National Standard (CNS) A4 specification (210 X 297 mm) A7 1278480 _B7_ V. Description of the invention (27) The weight of the physiological saline solution absorbed by the material other than the water absorbent resin (composition) 15 is determined, and the measured weight is regarded as a blank 値. The absorption capacity under load is calculated by the following formula: Absorption capacity under load (g/g) = (water absorption amount in blank within 60 minutes) / (weight of water-absorbent resin (composition) (g) ). (5) Analysis of chelating agent: The chelating agent is dissolved in water, and the total content of nitrogen triacetic acid (salt) in the chelating agent is analyzed by high performance liquid chromatography according to the following conditions: Liquid): 0·3 ml of 0.4 mol/L alum solution, 450 ml of 0·1N-KOH solution, 3 ml of 40% water-soluble tetra-n-butylammonium hydroxide solution, 3 ml of sulfuric acid, 2,5 50 ML of ice, 1.5 ml of Ethylene Glycol Ministry of Economics, Intellectual Property Office staff consumption cooperation 钍 printing (column): LichroCART 250-4 Superspher 100 RP-18e (4 A m), which is made by Merk (flow rate) ): 1 ml/min (detector): UV 2 5 8 nm (injection): 5 0 # 1 (6) Total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition: 1 g The water-absorbent resin composition was stirred in a physiological saline solution of 100 g for 1 hour, and then filtered, and the above-mentioned (5) liquid chromatography method was used to measure the nitrogen triacetic acid (salt) in the produced filtrate. Total 3α This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Ministry of Economics Intellectual Property The Bureau of Staff and Consumers Co., Ltd. printed B7____5, the invention description (28), to quantify the total content of nitrogen triacetate (salt) in the water-absorbent resin composition. (7) Evaluation method of discoloration of the water-absorbent resin composition over time: First, a distribution of 2,000 g of the water-absorbent resin composition (dry powder of the particle diameter of 600 to 300 //m unless otherwise noted) At the bottom of the polypropylene storage container (capacity 1 20 cc, Pack-Ace made by Ding 〇 ^ 〇 1 ^ company), the inner diameter of 5 5 111111 and the height of 7 〇 111111, and then at 70 ° C at 80% Under RH, it was allowed to stand for 5 days in a temperature and humidity regulator (PLTINOUS LUCIFER, model No. pL-2G, manufactured by Tabai Especk Co., Ltd.), and the container was not capped under the open system. Incidentally, the amount of distribution of the above water-absorbent resin composition per unit area (0 · 084 g/cm 2 ) is a high concentration core mode amount. After 5 days, the entire water-absorbent resin composition in the container was charged into a powder paste sample holder (30 mm 0 ) as follows, and the surface color of the water-absorbent resin composition was measured for the yellowing index. (YD is used under the setting conditions (reflex measurement/additional powder-paste sample holder (30 mm0)/powder-paste standard round whiteboard No.2/30 mm0 projection tube as standard), this system is used Spectroscopic color difference meter (SZ-Y-8 0 color measurement system, manufactured by Nippon Denshoku Kogyo Co., Ltd.) (8) Deodorization measurement (evaluation method for the proportion of disgusting odor): First, 5 g of water absorption The resin composition is placed in a closed polypropylene container (250 cc, Pack-Ace, manufactured by Teraoka), which is --- _ - λ1 · _ (please read the notes on the back before this page) .1^ (Re-booking-----------line
This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing -___B7__ five, invention description (29) 69mm opening diameter, 63mm bottom diameter, 97mm High, and 250 ml capacity. Next, 30 g of artificial urine can be further injected into the container, wherein 0.5 ml of the aqueous solution can be prepared by dissolving 15% of a water-soluble sodium methyl mercaptan solution (manufactured by Tokyo Kasei Kogyo Co., Ltd.). The unpleasant component was diluted 500 times with deionized water, and then the container was capped and sealed so that the gas did not leak out. The container was allowed to stand at 25 ° C, 5 5% RH for 4 hours, and then the concentration of methyl mercaptan in the container was measured using a detector, and the results were obtained as a representative of Gas Tech's detection tube. G 1. The detection tube used was Gas Tech's Ν ο 7 0 for all thiols (measuring range: 0 · 5 to 1 2 0 p p m ). The measurement is performed via the detection tube operation specified below. The detection tube system uses a single pumping (100 ml, 2 minutes) method. When the concentration measured therein is not more than 5 p pm, the pumping is performed 2 to 10 times, and the reading is divided by the number of pumping times. If the detection tube used is corrected with ethyl mercaptan, the concentration measurement is multiplied by the methyl mercaptan calculation factor of 0 · 7 (exhaustion times = 1). Next, the concentration of methyl mercaptan in the inner space of the container was measured in the same manner as above except that the water-absorbent resin composition and the artificial urine were not injected into the container, but an aqueous solution of 0.5 ml was injected, and the preparation was carried out by using deionized Water was diluted with 5% of a water-soluble sodium methyl mercaptan solution (manufactured by Tokyo Kasei Kogyo Co., Ltd.) by a factor of 500, and the result was referred to as G 0 . Then, the proportion of the disgusting odor is calculated by the following formula: The proportion of the disgusting odor (%) Please read the back of the note first.
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G〇-Gl)/G〇xl〇〇 Paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) ^2- A7 1278480 B7___ V. Description of invention (30) [Reference Example 1] Preparation 1 a water-soluble monomer solution, which comprises 67.0 parts of a 37% water-soluble sodium acrylate solution, 10.2 parts of acrylic acid, and 0. 979 parts of polyethylene glycol diacrylate (ethylene oxide unit) The average number: 8), and 22.0 parts of water are mixed together. Nitrogen is blown into the above water-soluble monomer solution in a large barrel, so that the dissolved oxygen concentration in the solution is lowered to not higher than 0.1 P P m . Then, the temperature of the above water-soluble monomer solution was adjusted to 18 ° C under nitrogen. Next, 0. 16 parts of 5% water-soluble sodium persulfate solution, 0. 16 parts of 5% 2,2 '-azobis(2-carbamidylpropane) dihydrogen chloride are dissolved under stirring. The solution, 0 · 15 parts of a 0.5 % L-ascorbic acid water-soluble solution, and 0 · 17 parts of 0.35% hydrogen peroxide water-soluble solution were added dropwise in that order. Printed by the Ministry of Economic Affairs Intellectual Property Office Staff Consumer Cooperative. Immediately after the dropwise addition of hydrogen peroxide, the polymerization reaction begins. Then, the stirring was stopped, and after 10 minutes, the temperature of the monomer reached a peak temperature. The peak temperature is 8 5 °C. Then, the vat was immersed in a hot water bath at 80 ° C and allowed to age for 10 minutes. The resulting clear water gel was crushed using a chopper and then dried at 180 ° C for 30 minutes. The resulting dried product was chopped using a mashing machine and then classified into a sieve passing through a 500 m sieve, but kept on a sieve of 10 5 /zm, thus obtaining a water-absorbent resin (A). It contains a solution of 0. 05 parts of ethylene glycol diglyceryl ether, 1 part of propylene glycol, 3 parts of water, and 1 part of isopropanol. This paper scale applies to China National Standard (CNS). A4 size (210 X 297 mm) 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printed B7_ V. Invention description (31) Mixing 100 parts of water-absorbent resin (A)' and the resulting mixture Heat treatment at 140 ° C for 40 minutes 'The surface-treated water-absorbent resin (B) was thus obtained. The results of measuring the physical properties of this surface-treated water-absorbent resin (B) are shown in Table 1 [Example 1] Under stirring, 60% sulfuric acid was added to a commercially available water-soluble penta-extension ethyl three. In the sodium pentaacetate solution (solid content: 40%), the p H range was adjusted from 1 to 8 to 2. The resulting solution was allowed to stand for a while, and then the deposited diethylenetriaminepentaacetic acid was filtered and then rinsed with pure water, and then dried at 60 °C. The total content of nitrogen triacetic acid (salt) in the above commercially available sodium hexaethyltriamine pentaacetate is about 5%, but the nitrogen triacetic acid in the produced di-ethyltriamine pentaacetic acid ( The total content of the salt was reduced to 35 p pm of the diethyltriamine pentaacetic acid via the above treatment. Adding 0. 05 parts of ethylene glycol diglyceryl ether to a diethylidene triamine pentaacetic acid having a total content of nitrogen triacetic acid (salt) obtained by the above-mentioned 0. a treatment solution prepared by using 1 part of propylene glycol, 3 parts of water, and 1 part of isopropyl alcohol, and mixing 1 part by weight of the water-absorbent resin (A) (as obtained in Reference Example 1), and The resulting mixture was heat-treated at 180 ° C for 40 minutes, thereby obtaining a water-absorbent resin composition (1) (wherein the mixing ratio of di-ethyltriamine pentaacetic acid was 20% of the water-absorbent resin (A) Ppm). &lt;Please read the notes on the back and fill in the ^page) 1 Order·----ΓΙ-——Line
This paper size applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm). 34 A7 1278480 _____B7_ V. INSTRUCTIONS (32) Measure the total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition ( 1). As a result, he accounts for 0.1 ppm or less of this composition and, therefore, is undetectable. The measurement results of the physical properties of the water-absorbent resin composition (1) are shown in Table 1. [Example 2] A water-absorbent resin composition (2) was obtained in the same manner as in Example 1, except that the amount of di-ethyltriamine pentaacetic acid in the treating agent solution was changed to 0 · 0 1 part ( The mixing ratio of diethyltriamine pentaacetic acid in the resulting composition is 1 〇〇ppm of the water-absorbent resin (A). 〇The nitrogen triacetic acid (salt) in the water-absorbent resin composition (2) is measured. The total content. As a result, he accounts for 0 · 1 p p m or less of this composition and, therefore, is unmeasurable. The measurement results of the physical properties of the water-absorbent resin composition (2) are shown in Table 1. [Example 3] Ministry of Economic Affairs, Intellectual Property Office, Staff Consumer Cooperative, printed by dissolving diethyleneethylamine pentaacetic acid (as obtained in Example 1) having a reduced content of nitrogen triacetic acid (salt) In water, a 0. 0 7% aqueous solution was prepared. 3 parts of this solution was sprayed; [〇〇 water-absorbent resin (B) (as obtained in Reference Example 1) and then dried at 80 ° C, thus obtaining a water-absorbent resin composition (3) (In which the mixing ratio of di-ethyltriamine pentaacetic acid accounts for 2 1 ppm of the water-absorbent resin (B)). This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 05-------------------------- A7 1278480 _____B7___ (Invention) (33) The total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition (3) was measured. As a result, he accounts for 0 · 1 P pm or less of this composition and, therefore, is undetectable. The measurement results of the physical properties of the water-absorbent resin composition (3) are shown in Table 1. [Example 4] A water-absorbent resin composition (4) was obtained in the same manner as in Example 3 except that the concentration of the water-soluble di-ethyltriamine pentaacetic acid solution was changed to 0 · 5% (in the resulting composition) The mixing ratio of di-ethyltriamine pentaacetic acid in the product is 1 500 ppm of the water-absorbent resin (B). The total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition (4) was measured. As a result, he accounts for 0. 1 ppm or less of this composition and, therefore, is unmeasurable. The measurement results of the physical properties of the water-absorbent resin composition (4) are shown in Table 1. [Example 5] The Ministry of Economic Affairs, the Intellectual Property Office, the employee consumption cooperative, printed a 0.1% aqueous solution, which had a di-ethyltriamine pentaacetic acid having a reduced content of nitrogen triacetic acid (salt). The one obtained in Example 1 was dissolved in water. A water-absorbent resin composition (5) obtained by performing the drying, mashing, and surface treatment steps in the same manner as in Reference Example 1, except that 3.5 parts of the above aqueous solution was added, and 100 parts were used in a chopper. The gel produced by the polymerization is crushed (in the gel, the mixing ratio of the diethyltriamine pentaacetic acid in the resulting composition is a solid content (essentially, the water-absorbent tree - -_• from - _ This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 _____ B7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing 5, invention description (34) fat) lOOppm). The total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition (5) was measured. The result 'the 占 · 1 p p m or less of this composition, therefore, is unmeasurable. The measurement results of the physical properties of the water-absorbent resin composition (5) are shown in Table 1. [Example 6] A method was prepared by mixing together sodium hydroxide, water, and di-ethyltriamine pentaacetic acid (as obtained in Example 1) having a reduced total content of nitrogen triacetic acid (salt) 3 5% water soluble tetrasodium diethyltriamine pentaacetate solution. The aqueous solution was diluted 200 times with water. 3 parts of this diluted solution was sprayed to 1 part by weight of the water-absorbent resin (B) (as obtained in Reference Example 1) to prepare a mixture, and then heated at 80 ° C. Thus, a water-absorbent resin was obtained. The composition (6) (wherein the mixing ratio of sodium tetraethylammonium pentaacetate is 5 2 · 5 ppm of the water-absorbent resin (B)). The total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition (6) was measured. As a result, he accounts for 0 · 1 p pm or less of this composition, and therefore, is unmeasurable. The measurement results of the physical properties of the water-absorbent resin composition (6) are shown in Table 1. [Example 7] 3 parts of a diluted solution (as obtained in Example 6), 0. 05 parts of ethylene glycol diglyceryl ether, 1 part of propylene glycol, and __-________ · 27 were included therein. (Please read the notes on the back and fill in the ^4 page) #填填,——^-----线
V The paper size applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) A7 1278480 ___ B7___ V. Inventive Note (35) The water-absorbent tree is mixed with the water-absorbent resin sodium. For the physical properties of triacetic acid (salt ρ pm or lower), please read Ϊ Back Sr Note: 1 page of isopropyl alcohol treatment solution, mixed with 1 〇〇月(A) (as in The compound obtained in Reference Example 1 was heated and treated at 180 ° C for 40 minutes, thereby obtaining a composition (7) (wherein tetraethylammonium triamine pentaacetic acid was used as the water absorbent resin (A) 5 2 · 5 ppm ). The total content of nitrogen in the water-absorbent resin composition (7) was measured. As a result, he accounts for 0.1 of this composition and, therefore, is unmeasurable. The water-absorbent resin composition (the measurement results of the quality are shown in Table 1. [Example 8] Sixty percent of sulfuric acid was added to a commercially available solution of water-soluble hexamethyleneethyltetraamine hexaacetate (solid) under stirring. In the content: 40%), the pH is adjusted to be in the range of 1.8 to 2 Torr, and the resulting solution is allowed to stand for a while, and then the deposited tri-ethyltetramine hexaacetic acid is filtered and then rinsed with pure water, and Then dried at 60 ° C. The Ministry of Economic Affairs, Intellectual Property Bureau, Staff Cooperatives, printed in the produced tri-ethyltetramine hexaacetic acid, the total content of nitrogen triacetic acid (salt) accounted for triethylammonium hexaacetate 2 0 P pm. Prepare a 35 % water-soluble three-stretch by mixing sodium hydroxide, water and the above-mentioned tri-extended ethyltetraamine hexaacetic acid having a reduced content of nitrogen triacetic acid (salt) Ethyltetraamine hexaacetic acid pentasodium solution. The aqueous solution was diluted 200 times with water. 3 parts of this diluted solution was sprayed to 1 part of water-absorbent resin (B) (as obtained in Reference Example 1) ) to make a mixture, and then -3S- paper scale for Chinese countries Standard (CNS) A4 size (210 X 297 mm) A7 1278480 B7_ V. Description of invention (36) Heating at 80 ° C, thus obtaining a water-absorbent resin composition (8) (wherein the mixing ratio is tri-extension ethyl four The pentasodium amine hexaacetate accounts for 5 2 · 5 P pm of the water-absorbent resin (B). The total content of nitrogen triacetic acid (salt) in the water-absorbent resin composition (8) is measured. The measurement results of the physical properties of the water-absorbent resin composition (8) are shown in Table 1. [Comparative Example 1] The same as in Example 2, the measurement was not possible. By way of comparison, the water-absorbent resin composition (1) is obtained, except that di-ethyltriamine pentaacetic acid having a total content of nitrogen triacetic acid (salt) is substituted with an aqueous solution, and the preparation of the aqueous solution can be commercially available. The sodium hexaacetate pentaacetate is obtained by dissolving it in water in the original form. The total content of nitrogen triacetic acid (salt) in the comparative water absorbing resin composition (1) accounts for the composition. 5 ρ P m. Comparison of physical properties of water-absorbent resin composition (1) The results are shown in Table 1. [Reference Example 2] A water-soluble monomer solution prepared by using 76 parts of a 37% water-soluble sodium acrylate solution, 7 parts of acrylic acid, and 5 parts of polyethylene glycol. The diacrylate (the average number of ethylene oxide units: 8) and 15 parts of water are mixed together. The paper scale applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) l· I ! II *1 II Γ I ! - {Please read the notes on the back and fill in 3 pages)
Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumer Cooperatives, Printing 1278480 A7 Ministry of Economic Affairs, Intellectual Property Bureau, Staff and Consumer Cooperatives Printing _ B7___ V. Invention Description (37) In a double-arm kneading machine with a protective cover, nitrogen is blown into the above A water soluble monomer solution that removes dissolved oxygen from the solution. Then, the temperature of the water-soluble monomer solution was adjusted to 22 °C. Next, with stirring, 1 part of a 5% aqueous sodium persulfate solution and 0. 0 4 parts of a water-soluble solution of 0.5% L-pithalosic acid were added. One minute after this addition, the water-soluble monomer dissolved in a mist and the temperature began to rise. After another 20 minutes, the temperature reached a peak temperature, and then the solution was aged for 20 minutes with stirring. This peak temperature is at 9 4 °C. After the end of aging, the resulting gel was taken out and then dried at 170 ° C. The dried polymer produced was honed and then classified as passing through a sieve of 850 //m, but kept The water-absorbent resin (C) was thus obtained on a sieve of 1 〇 5 /zm, which contained 0.05 parts of ethylene glycol diglyceryl ether, 1 part of propylene glycol, 3 parts of water, and 1 part of a difference. a composition solution of propanol, mixed with 100 parts of the water-absorbent resin (C), and the resulting mixture was heat-treated at 180 ° C for 40 minutes, thereby obtaining a surface-treated water-absorbent resin (D). The physical property measurement results of this surface-treated water-absorbent resin (D) are shown in Table 1. [Example 9] By adding sodium hydroxide, deionized water and having a reduced total content of nitrogen triacetic acid (salt) The di-ethyltriamine pentaacetic acid (as obtained in Example 1) was mixed together to prepare a 35% water-soluble tetra-diethylethylamine penta-wood paper scale applicable to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) (Please read the notes on the back and fill in the page): Fill in..——^----- line
-40- A7 1278480 ____B7_______ V. Description of the invention (38) Sodium acetate solution. This aqueous solution was diluted 200 times with deionized water, and then 3 parts of this diluted solution was sprayed to 100 parts of the water-absorbent resin (D) (as obtained in Reference Example 2) to prepare a mixture. And then heating at 80 ° C, thus obtaining a water-absorbent resin composition (9) (wherein the mixing ratio of sodium tetraethylammonium pentaacetate is 52.5 ppm of the water-absorbent resin (D)) 〇 measurement The total content of nitrogen triacetic acid (salt) in the water absorbent resin composition (9). As a result, he accounts for 0.1 ppm or less of this composition, and therefore, is unmeasurable. The measurement results of the physical properties of the water-absorbent resin composition (9) are shown in Table 1. [Comparative Example 2] Printing by the Ministry of Economic Affairs, Intellectual Property Office, Staff Consumer Cooperative, the commercially available sodium salt of sodium succinate and sodium triamine pentaacetate as used in Example 1 was diluted 200 times with deionized water. 3 parts of this diluted solution was sprayed to 100 parts of the water-absorbent resin (D) (as obtained in Reference Example 2) to prepare a mixture, and then heated at 80 ° C, thus obtaining a comparative water-absorbent resin. Composition (2). The total content of nitrogen triacetic acid (salt) in the comparative water-absorbent resin composition (2) was 3 p p m of this composition. The physical property measurement results of the comparative water-absorbent resin composition (2) are shown in Table 1. (Comparity of light resistance) In a polypropylene container, a water-absorbent resin composition (9), a comparative water-absorbent resin composition (2), and a water-absorbent resin (D) (minutes -^44--this paper) The scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printing __B7__ V. Invention description (40) Then deposited diethylene ethylamine The acetic acid is filtered and then rinsed with pure water, and then dried at 60 ° C. The total content of nitrogen triacetic acid (salt) in the resulting di-ethyltriamine pentaacetic acid is 0 · 1 ppm or less, The diethyltriamine pentaacetic acid is therefore undetectable. A solution of a 35% water-soluble tetrasodium diethylammonium pentaacetate solution is prepared by using sodium hydroxide, deionized water and the like. Diethylidene triamine pentaacetic acid, which reduces the total content of nitrogen triacetic acid (salt), is mixed together. The aqueous solution is diluted 200 times with deionized water. 3 parts of this diluted solution is sprayed to 100 parts. Water-absorbent resin (B) (as obtained in Reference Example 1) to make a mixture, And then heating at 80 ° C, thus obtaining a water-absorbent resin composition (10) (wherein the mixing ratio of tetraethylammonium triamine pentaacetate to the water-absorbent resin (B) was 52 · 5 ppm). The total content of the nitrogen triacetic acid (salt) in the water-absorbent resin composition (10). As a result, it accounts for 0.1 ppm or less of the composition, and therefore, is undetectable. The water-absorbent resin composition ( The measurement results of the physical properties of 10) are shown in Table 1. [Example 1 1] A water-absorbent resin composition (1 1 ) was obtained in the same manner as in Example 10 except that the water-absorbent resin (B) was used. (as obtained in Reference Example 1) was replaced with a water-absorbent resin (D) (as obtained in Reference Example 2) (in the resulting composition, di-ethyltriaminepentaacetate tetrasodium (please first) Read the notes on the back and fill in @页) · · Order, ——^-----Line
This paper scale applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) 4a A7 1278480 B7 _ V. The invention (41) has a mixing ratio of 5 2 · 5 p p m of the water-absorbent resin (D). The total content of nitrogen triacetic acid (salt) in the water absorbent resin composition (1 1 ) was measured. As a result, he accounts for 0.1 ppm or less of this composition and, therefore, is undetectable. The measurement results (1 1 ) of the physical properties of the water-absorbent resin composition are shown in Table 1. [Example 1 2] A water-absorbent resin composition (1 2 ) was obtained in the same manner as in the preparation of the water-absorbent resin composition (10) in Example 10 except that: a water-soluble deodorant (a 15% aqueous solution of Camellia leaf extract), which will be present in an aqueous solution at a concentration of 16.7% and diluted by 200 times; 3 parts of the resulting aqueous solution is sprayed to 1 0 parts of the water-absorbent resin (B) (as obtained in Reference Example 1) to prepare a mixture, and then heated at 80 ° C; and then heated in the mixture, added in a ratio of 0.5% An inorganic powder containing cerium oxide (Aerosil 2000 manufactured by Nippon Aerosil Co., Ltd.). Printed by the Intellectual Property Office of the Ministry of Economic Affairs, Employees' Consumer Cooperatives [Example 1 3] As in the same preparation method as in Example 10, the water-absorbent resin composition (1 〇), a water-absorbent resin composition (1 3 ) was obtained, except: An aqueous solution is prepared by using a commercially available water-soluble deodorant (a 15% aqueous solution of Camellia leaf extract), which is present in an aqueous solution at a concentration of 16 · 7% and diluted by 200 times; 3 copies of this paper scale apply to China National Standard (CNS) A4 specification (210 X 297 mm) A7 Ministry of Economic Affairs Intellectual Property Bureau Staff Consumer Cooperative Printed 1278480 B7____ V. Invention Description (42) The resulting aqueous solution is mixed to 1 〇 A portion of the water-absorbent resin (D) (as obtained in Reference Example 2). [Example 14] As in the preparation method of the water-absorbent resin composition (1 〇) of Example 1, the water-absorbent resin composition (1 4 ) was obtained except that an aqueous solution was prepared by using a commercially available water-soluble solution. Deodorant (Oaklean EX is manufactured by TAIYO K0RY0), which will be present in an aqueous solution at a concentration of 16 · 7% and diluted by 200 times; 3 parts of the resulting aqueous solution is sprayed to 100 parts of water. The resin (B) (as obtained in Reference Example 1) was mixed together. [Example 1 5] A water-absorbent resin composition (15) obtained by adding a commercially available water-soluble deodorant (Eporion manufactured by Aiko Co., Ltd.) to a water-repellent resin composition of 10 parts by weight (1 0) ) (as obtained in Example 1), the ratio is 0 · 5 %, so that the two are mixed together. This paper scale applies to China National Standard (CNS) A4 specification (210 X 297 mm) 1278480 A7 B7 43 /V Ming Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printed f # S mmm 锬@汩«伫驺m ^ 1 1 • 1 1 1 1 1 1 1 1 1 • OO CM 1 JO m wn Yellowing index (YD after test 1 oo 2 1 1 • I 1 1 1 OO v〇cn 1 inch cn &lt;N r- oj Cn « 1 1 1 1 1 Before the test 1 vo CM rn 1 2 inch 1 1 1 1 1 « Light resistance (%) 1 • 1 1 1 I 1 1 I 1 ΓΝ m 沄I 1 Lu 1 1 1 sa 苤锑m cn m cn m cn cn m cn m cn cn cn cn cn m cn OO cn oo m oo cn m cn OO OO oa OO cn cn cn cn cn S 'Sb wT &gt;W^ 顺;_ . c£娣汔荽5 ® CN 〇\ CN oo CM s R 04 ON CN R oo CM S s rs S 1 1 1 1 Dissolution degradation extractable content (%) &lt;N inch oa JO - 2 OJ oa to CO Oo 2 OJ oo 04 OO Oi OJ leaching extractable content (%) 2222 2222 v 〇 2 VO 2 VO 2 VO bis 2 oz Ofl mi ci JO ; 〇s JO Water-absorbent resin (composition) ) B yv δ δ δ gg Compare (1) δ Compare (2)! s /-N 2 £ (Please read the notes on the back and fill in the 0^4 page). Order /---;-----Line
SN (C standard country paper with a moderate ruler paper PCT 97 2 X 10 (2 stipulated 1278480 A7 _____ Β 7_ V. Illustrative (44) Various details of the invention may be changed without departing from the spirit or scope thereof. In addition, the foregoing description of the preferred embodiments of the present invention are intended for the purpose of illustration Bureau employees' consumption cooperatives print the paper scale applicable to China National Standard (CNS) A4 specification (210 X 297 mm)
1278480 A8 一B8~~ r—-公-告表--- VI. Application for Patent Scope--- Patent Application No. 89 126490 Revision of Chinese Patent Application Revision of the Republic of China on December 29, 1995 1 · A granular form a water-absorbent resin composition comprising a water-absorbent resin and an aminoacetic acid chelating agent, wherein a mixing ratio of the aminoacetic acid chelating agent in the water-absorbent resin composition is not less than 1 〇ppm of the water-absorbent resin, and the water absorbing property thereof The total content of the nitrogen triacetic acid and the salt thereof in the resin composition is not more than 1 ppm of the water absorbent resin composition, and the ratio of the water absorbent resin to the particulate water absorbent resin composition is not less than 75% by weight. 2 . A particulate water-absorbent resin composition comprising a water-absorbent resin and an aminoacetic acid chelating agent, wherein the total content of the nitrogen triacetic acid and the salt thereof is not more than the aminoacetic acid chelating agent in the water-absorbent resin composition 1,0 0 0 PP m, wherein the water-absorbent resin accounts for not less than 75% by weight of the particulate water-absorbent resin composition. 3. The water-absorbent resin composition of claim 1, which further comprises a water-soluble deodorant. 4. The water-absorbent resin composition of claim 2, which further comprises a water-soluble deodorant. 5. The water-absorbent resin composition of claim 1, wherein the absorption capacity under no load is not less than 30 g / g, and the deteriorated extractable content of the elution is not more than 20% by weight. The absorption capacity under the load of 1 · 9 k P a is not less than 28 g / g, and the yellowness index is not more than 26 . 6. For the water-absorbent resin composition of the second paragraph of the patent application, the paper size of the exhibition shall be in accordance with the Chinese National Standard (CNS) A4 specification (210X297 mm) (please read the notes on the back and fill in this page) _n^ · Ministry of Economic Affairs Intellectual Property Bureau employee consumption cooperative printed 1278480 A8 B8 C8 D8 VI. Application for patent scope (please read the first ## note on the back and fill in this page) The absorption capacity under no load is not less than 30 g / g, the deteriorated extractables content of the dissolution is not more than 20% by weight, the absorption capacity under the load of 1. 9 kPa is not less than 28 g/g, and the yellowing index is not higher than 26. 7) The water-absorbent resin composition of claim 3, which exhibits an absorption capacity of not less than 30 g / g under no load, and a degraded extractable extract content of not more than 20% by weight, The absorption capacity under the load of 1. 9 kPa is not less than 28 g/g, and the yellowing index is not higher than 26. 8) The water-absorbent resin composition of claim 4, which exhibits an absorption capacity of not less than 30 g / g under no load, and a degraded extractable extract content of not more than 20% by weight, The absorption capacity under a load of 1.9 kPa is not less than 28 g/g, and the yellowness index is not higher than 26. 9. The water-absorbent resin composition according to claim 1 or 2, which further comprises a water-soluble deodorant, and exhibits an absorption capacity under no load of not less than 30 g / g, deterioration of dissolution The extractables content is not more than 20% by weight, the absorption capacity under the load of 1.9 kPa is not less than 28 g / g, and the proportion of the disgusting odor is not less than 40%. Printed by the Intellectual Property Office of the Ministry of Economic Affairs, the Consumers' Cooperatives. 1 • The water-absorbent resin composition of the first application of the patent scope, wherein the water-absorbent resin is partially neutralized and crosslinked poly(acrylic acid), derived from polymeric hydrophilicity. A monomeric process wherein the monomer comprises a monomer component having a major proportion selected from the group consisting of acrylic acid, acrylate salts, and mixtures thereof. 1 1 The water-absorbent resin composition of claim 2, wherein the water-absorbent resin is a partially neutralized and crosslinked poly(acrylic acid) obtained by a method of polymerizing a hydrophilic monomer, and the monomer is A monomer component comprising a major proportion selected from the group consisting of acrylic acid, acrylate salts, and mixtures thereof. -2 - The paper size is based on the Chinese National Standard (CNS) A4 specification (210X297 mm) 1278480 Δ8 Α8 Β8 C8 _D8 ______ VI. Patent application scope 1 2 ·If the water absorption tree of claim 9 is composed of 3 Where the water-absorbent resin is a partially neutralized and crosslinked poly(acrylic acid) obtained from a method of polymerizing a hydrophilic monomer, and the monomer comprises a monomer selected from the group consisting essentially of acrylic acid, acrylate, and mixtures thereof. ingredient. 1 3 . The water-absorbent resin composition as claimed in claim 1 or 2 is used as a sanitary material. A use of a water-absorbent resin composition as claimed in claim 1 or 2 for the production of sanitary materials. (Please read the notes on the back and fill out this page.) Printed by the Intellectual Property Office of the Ministry of Economic Affairs. Employees' Consumption Cooperatives Printed in this paper, the Chinese National Standard (CNS) Α4 specification (210X297 mm) · 3 -
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