Abstract: The present invention relates to: a super-absorbent polymer having excellent basic absorption performance and also being capable of improving rewetting characteristics and leakage suppression characteristics of a sanitary product such as diapers; and a preparation method therefor. The super-absorbent polymer comprises: a base resin powder comprising a first cross-linked polymer of a water-soluble ethylenically unsaturated monomer having an acidic group of which at least a part is neutralized; and a surface cross-linked layer comprising a second cross-linked polymer in which the first cross-linked polymer is additionally cross-linked with a surface cross-linking agent as a mediator wherein the surface cross-linking agent comprises a mixture of multiple types of cyclic alkylene carbonates and the mixture has a Hansen solubility parameter due to a hydrogen-bonding component of 13 or greater.
The present invention is basic absorption performance as well as excellent, the present invention relates to diapers such as sanitary material rijjat (rewet) characteristics and high to improve the leakage suppression characteristics and a method of manufacturing a water-absorbent resin.
[Background Art]
The superabsorbent resin (Super Absorbent Polymer, SAP) field 500 to its own weight
1, a synthetic polymer material that has the ability to absorb moisture of about a thousand times, every developer has named each with a different name, such as SAM (Super Absorbency Material), AGM (Absorbent Gel Material). Superabsorbent polymer as described above is to begin commercialization of physiological equipment, currently freshness at Children diapers, etc. sanitary ware in addition to horticultural soil repair filler, engineering, construction index material, nursery sheets, food for distribution areas first, and It has been widely used for a material such as a poultice.
In most cases, these high water-absorbent resin has there been widely used in hygienic material fields, such as diapers and sanitary napkins, for this purpose it is necessary to exhibit a high absorption capacity for such as moisture, high pressure that the absorbed moisture to the outside pressure not get out and it is necessary to exhibit the ability to absorb the like.
In addition, the super-absorbent resin has, need to be wide as much as possible diffusion of the urine, etc. When included in the sanitary material such as a diaper. This allows, by utilizing the super-absorbent resin particles included in the area around the absorbent layer of the sanitary material as a whole can be further improved hygiene material absorbing performance and absorption rate. In addition, due to such a diffusion characteristic, one high and the urine etc. was absorbed by the water-absorbent resin can be further improved riswet (rewet) characteristics of the diaper to prevent the coming out of the bare again, the same time makes it possible to improve the leakage suppression characteristics of the diaper do.
Previously, by changing the design, such as sanitary material such as the diaper itself, the urine
The improvement of the properties of widely spread mainly attempts. For example, a sanitary material
Introducing ADL (Acquisition Distribution Layer) or the like, and the method by utilizing the absorption channel rounded, the ways to improve the diffusion characteristics, such as the urine attempt bar. However, the improvement was due to a design change in the diffusion properties of these hygiene material itself is not enough, there is a continuing requirement to further improve on this.
[Detailed Description of the Invention]
[SUMMARY]
The present invention, as well as to be excellent in the basic absorption performance, high water-absorbent resin and that was widely spread the own urine, etc. to improve properties of improve the hygiene material rijjat (rewet) characteristic and leakage suppression characteristics absorbent resin and a method to provide.
[Technical Solution]
The present invention is a base resin powder including a first cross-linked polymers of water soluble ethylenically unsaturated monomer having an acid group at least partially jeunghwa; And
A super-absorbent resin to the first cross-linked polymer is formed on the base resin powder, a cross-linked layer includes a surface including a second cross-linked polymer cross-linking a surface cross-linking agent is added to the medium,
The surface cross-linking agent is 13 or more and a water-absorbent resin Hansen solubility parameters (Hansen solubility parameter) by including a common compound of cyclic alkylene carbonate in a plurality of types, and wherein the common compound is the hydrogen bonding component (hydro ^ n bonding component) to provide.
The present invention also comprising the steps of: in the presence of an internal crosslinking agent, to form a hydrogel polymer comprising a first cross-linked polymer by cross-linking polymerization of the water-soluble ethylenically unsaturated monomer having at least partially neutralized acid;
Forming a function of the gel polymer dried, pulverized and classified to a base resin powder; And
In the presence of a surface cross-linking agent, and including the step of surface crosslinking by heating a base resin powder,
The surface cross-linking agent comprises a common compound of cyclic alkylene carbonate in a plurality of types, and wherein the common compound A method of manufacturing a super-absorbent resin having a Hansen solubility parameters (Hansen solubility parameter) by the hydrogen-bonding component (hydrogen bonding component) 13 It provides.
Hereinafter, there will be more fully describes the collection of specific embodiments and the water-absorbent resin and its production process according to the invention. However, it is to be presented as an illustration of the invention and thus is not limited by the scope of the invention, it is apparent to those skilled in the art are possible are various modifications to the embodiments within the scope of the invention. Additionally, "including" Unless otherwise noted in this specification, or
Box "containing" refers to la are including without limitation any component (or components) can not be construed to exclude the addition of other component (or components).
According to one embodiment of the invention, the base resin powder including a first cross-linked polymers of water soluble ethylenically unsaturated monomer having at least partially neutralized acid; And
A super-absorbent resin to the first cross-linked polymer is formed on the base resin powder, a cross-linked layer includes a surface including a second cross-linked polymer cross-linking a surface cross-linking agent is added to the medium,
The surface cross-linking agent comprises a common compound of cyclic alkylene carbonate in a plurality of types, and wherein the common compound is provided with a super-absorbent resin having a Hansen solubility parameter of hydrogen bonding component 13.
As a common compound, including the continuous experiments, specific surface cross-linking agent common compound, i.e., a cyclic alkylene carbonate in a plurality of kinds of the inventors of the present invention, proceed to the surface cross-linked by the Hansen solubility parameters according to the hydrogen bond component using a common compound more than 13 but as a result, it remains excellent basic absorption performance of the superabsorbent polymer, superabsorbent polymer that itself is capable to quickly and widely diffuses the urine, etc. absorbed by the hygienic material improves the hygiene material riswet (rewet) characteristic and leakage suppression characteristics this was confirmed.
This cyclic alkylene carbonate in a plurality of types are the following principles
It is estimated to be because they can lead to synergistic. In order for the Hansen solubility parameter of hydrogen bonding component of water the heunhap is over 13, with ethylene carbonate or a first cyclic alkylene carbonates such as propylene carbonate, the release of this widely used as a surface cross-linking agent before, Hansen due to the hydrogen bond component the solubility parameter is the number of the second cyclic alkylene carbonate is used, such as the glycerides that are very high as 15 or more, or 16 or more carbonates.
First, the ethylene carbonate or the first cyclic alkylene carbonates such as propylene carbonate is known to have an excellent surface crosslinking properties, and uses it to the basic performance of the water-absorbent resin (e.g., high pressure, absorption capacity or the whole liquid including ) it can be excellently expression. In addition, of the Hansen solubility absorbing resin particles the parameter is higher second cyclic alkylene carbonate and can give hydrophilicity to the surface of the water absorbent resin particles, whereby the like absorbed urine in the sanitary material and due to the hydrogen bond component It can be quickly and widely spread along the surface. As a result, one embodiment superabsorbent polymer, as well as receive it excellent in basic absorption performance or barrel-component, to spread widely and the like absorbed urine in sanitary material to improve the hygiene material rijjat (rewet) characteristic and leakage suppression characteristics can.
Hereinafter, one embodiment that will be described in more detail on the water-absorbent resin ■ it.
As referred to herein, "superabsorbent polymer, is a base resin powder including a first cross-linked polymers of water soluble ethylenically unsaturated monomer having at least partially neutralized acid; And that means the water absorbent resin including the resin powder is formed on the base, wherein the added crosslinked with a surface cross-linked layer, including two cross-linked polymer with the surface cross-linking agent intermediate the first cross-linked polymer.
The water-soluble ethylenically unsaturated monomer may be any monomer that is commonly used in the manufacture of a superabsorbent polymer. Non-limiting examples of the water-soluble ethylenically unsaturated monomer may be a compound represented by the following general formula (1):
Formula 1
R COOM1
In the formula 1,
^ Is an alkyl group of 2 to 5 carbon atoms including an unsaturated bond,
M 1 is a hydrogen atom, or one divalent metal, an ammonium group or an organic amine salt. Suitably, the monomer may be at least one member selected from acrylic acid, methacrylic acid, and monovalent metal salts of these acids, the group consisting of a divalent metal salt, ammonium salt and organic amine salt. Thus, when using an acrylic acid or a salt of a water-soluble ethylenically unsaturated monomer advantageously superabsorbent improved to obtain a water-absorbent resin. In addition, one-propanesulfonic acid in the monomer to maleic anhydride, fumaric acid, crotonic acid, itaconic acid, ethanesulfonic acid one by one ethanesulfonic acid, 2-methacryloyloxyethyl 2-acrylate, 2- (meth) acrylate, or 2- ( meth) anionic acrylamide-2-methylpropanesulfonic acid monomer and its salts; (Meth) acrylamide, N- substituted (meth) acrylate, 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, methoxy polyethylene glycol (meth) acrylate or polyethylene glycol ( meth) non-ionic hydrophilic monomers containing acrylate; And (Ν, Ν)-dimethylaminopropyl (meth) an amino group-containing unsaturated monomer of acrylamide and their quaternary cargo-dimethylaminoethyl (meth) acrylate or (Ν, Ν); at least one selected from the group consisting of It can be used.
Here, the water-soluble ethylenically unsaturated monomer having an acidic group, may be at least partially neutralizing the acid groups. Preferably it is used which is partially neutralized the monomers with an alkali substance such as sodium hydroxide, potassium hydroxide, ammonium hydroxide.
In this case, the neutralization degree of the monomer is 40 to 95 mole 0 / 0 , or 40 to 80 mole 0 / 0 may be, or 45 to 75 mol%. Range of the degree of neutralization may be different depending on the final physical properties, the degree of neutralization precipitation is too high, the neutralized monomer may be difficult to polymerization proceeds smoothly, whereas if the degree of neutralization is too low, as well as degrade the polymeric absorbent significantly difficult to handle elastic " it may represent a property, such as rubber.
In one embodiment said set absorption resin, the "first crosslinked polymer" refers to a water-soluble ethylenically unsaturated monomer described above the presence of the internal cross-linking agent to cross-linking polymerization
It means, and the "base resin powder is, and this to mean a material comprising a first crosslinked polymer. In addition, the 'means that the second crosslinked polymer is, more cross-linked material by cross-linking the first polymer is a parameter, and the surface cross-linking agent, a cross-linked surface layer containing them is formed on the base resin powder.
In the superabsorbent polymer said one embodiment, bran contained in the base resin powder U cross-linked polymer is a poly (meth) acrylates and C 2 of ¾ rheology of a carbon number of 8-bis (meth) acrylamide to 12, 2 to 10 carbon atoms to from the group consisting of poly (meth) allyl ethers of polyols of 10 in the presence of at least one kinds selected internal cross-linking agent, the above-mentioned monomer may be polymerized as a crosslinked polymer. More specific examples of the inner crosslinking agent is not particularly limited, teurimetilreul tri (meth) acrylate, ethylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, propylene glycol di (meth) acrylate, polypropylene glycol di (meth) acrylate, butane diol di (meth) acrylate, butylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, acid di (meth) acrylate, tree, the ethylene glycol di (meth) acrylate, tripropylene glycol di (meth) acrylate, tetraethylene glycol di (meth) acrylate, di-penta the EPO Li pentaacrylate, glycerin tri (meth) acrylate or a penta-erythro and tetra-acrylate or the like, in addition to that of the water-absorbent resin Article may be used without limitation in a variety of internal cross-linking agent known to be possible.
In addition, in one embodiment the super-absorbent resin, a second cross-linked polymer with the surface cross-linked layer may be a crosslinked polymer with a first cross-linking polymerization mentioned above add a specific surface cross-linking agent in the polymer medium. In particular, in the high water-absorbent resin In some embodiments, using a surface crosslinking agent containing a plurality of kinds of common compounds cyclic alkylene carbonate to form a second cross-linked polymer and the surface cross-linked layer.
At this time, the surface cross-linking agent of the common compounds status may indicate the Hansen Solubility Parameter (Hansen solubility parameter) is 13 or higher, or 14 to 18 or 14.5 to 16.0 in characteristics due to the hydrogen bonding component (hydrogen bonding component).
The common compounds and Hansen of cyclic alkylene carbonate to be contained therein
Solubility parameter "CM Hansen," Hansen Solubility Parameters; A User's Handbook can be identified and calculated according to the method described in ", CRC Press, 2nd ed. (2012)". More specifically, according to the above document, the Hansen solubility parameters of some components may be respectively identified as due to the dispersion (dispersion force), polar forces (polar force) and a hydrogen bonding component (hydrogen bonding component), one embodiment and water-absorbent resin via the Hansen solubility parameter according to the hydrogen bond component among these three Hansen solubility parameters, will define the surface cross-linking agent.
That is, how each cyclic alkylene, respectively calculate the Hansen solubility parameter of hydrogen bonding component of the carbonate, and after checking, the content of each of the cyclic alkylene carbonate on the basis of (% by weight) contained in the common compounds according to the described in the above literature as a weight average value of the parameter value can be determined by the value of Hansen solubility parameter hydrogen bonding component of the surface cross-linking agent of the common state compounds.
These parameter values may define a hydrophilic range having a surface cross-linking agent of the common compound state, in accordance with experimental results of the inventors, having a Hansen solubility parameter according to the common compounds state of the surface cross-linking agent is a hydrogen bonding component of 13 Accordingly, one embodiment and while maintaining the excellent absorption performance, and barrel-component water-absorbing resin, and are given the appropriate hydrophilicity to the surface of the water absorbent resin particle (for example, a surface cross-linked layer surface), such as sanitary jaesse absorbed urine and along the surface of the water absorbent resin particles can be quickly and widely spread. As a result, the sanitary material such as diapers riswet (rewet) suppressing characteristics and leakage characteristics can be greatly improved.
On the other hand, to the surface cross-linking agent comprising a common compound of the plural kinds of cyclic alkylene carbonates of the above to have a Hansen solubility parameter by more than 13 hydrogen bond component, wherein the surface cross-linking agent is the Hansen solubility parameter according to the hydrogen bond component 10 and a first cyclic alkylene carbonate to 13, the Hansen solubility parameters according to the hydrogen bond component can contain an alkylen carbonate-type second ring of 16 to 20 together.
Of these, the first cyclic alkylene carbonate may be secured and the like basic ability to absorb and / or barrel-component of the water absorbent resin, and the like and specific examples thereof include ethylene carbonate or propylene carbonate. In addition, the second cyclic alkylene carbonate is a high hydrophilicity to the surface of the water absorbent resin particles
As a component for imparting to improve the hygiene material riswet (rewet) suppressing properties and leakage properties, and specific examples thereof include and the like glyceryl carbonate.
These first and second cyclic alkylene carbonate is 0.9 : 1 to 1: indicating the may be included in the surface cross-linking agent in a weight ratio of 2, This allows, one embodiment and the water-absorbent resin more excellent absorption performance and / or barrel-component also and the like, hygienic material riswet (rewet) suppressing characteristics and leakage characteristics can be further improved.
On the other hand, the above-described one embodiment and the water absorbent resin may have a particle size of 150 to 850. More specifically, the base resin powder and having at least and less than 95% by weight of particle diameter of 150 to 850 of the water-absorbent resin containing them, a fine powder having a particle size of less than 150 ΛΙΙ be less than 3% by weight.
The example super-absorbent resin wherein an implementation is excellent in basic performance and no pressure to absorb liquid tube, which may be defined by the physical properties such as CRC and GBP. Specifically, in one embodiment the superabsorbent resin is a saline solution (0.9 weight 0 / 0 by centrifugation beam SAT (CRC) is 27 to 37 g / g, or 28 to 32 g / g in 30 minutes for the sodium chloride solution) It can be. This centrifugation beam SAT (CRC) range may define a pressureless excellent absorption performance and high-absorbent resin that indicates an implementation example.
Centrifugation beam SAT (CRC) for the physiological saline solution is then absorbed by the saline solution through the superabsorbent polymer in 30 minutes can be calculated by the following formula 1 of:
[Equation 1]
CRC(g/g) = {[W2(g) - W!(g) - Wo(g)] W0(g)}
In the formula 1,
W 0 (g) is the initial weight (g) of the superabsorbent resin,
And W ^ g) is the weight measured after then impregnated for 30 minutes in physiological saline, dehydrated by using a centrifuge 3 minutes at 250G the nonwoven envelope without inserting the superabsorbent polymer at room temperature,
W 2 (g) is a weight measured after one and after the non-woven fabric into an envelope an absorbent resin impregnated for 30 minutes in physiological saline at room temperature, dehydrated by using a centrifuge 3 minutes at 250G.
Further, one embodiment the superabsorbent resin is a gel bed permeability (GBP) of the physiological saline 23 darcy or more, or 23 to 35darcy, black is 26 to fattening it is subject to a 32 darcy, which has an example super-absorbent resin implementation you can define a good through liquid.
Gel bed permeability (GBP) of the physiological saline is Darcy (Darcy) or cin in accordance with the following method described in Korea Patent Application No. 10- 2014-7018005 No. 2 can be measured in units of. 1 darcy is meant to flow the first 1 mm per second through the liquid with a viscosity of lcP lcuf under a pressure gradient of one atmosphere per 1cm. Gel bed permeability has the same units as area 1 darcy is 0.98692 χ 10 "12 m 2 or 0.98692 10 " 8 are as ciif. Means more specifically, GBP is penetrated to the gel layer (or bed) it swelled under the conditions called free-swelling conditions of Opsi also (or transmittance) (Gel Bed Permeability (GBP) Under Opsi Swell Pressure Test) herein, and the GBP can be measured using the apparatus as shown in the figure above the arc Korea Patent Application No. 10-2014-7018005.
On the other hand, an implementation example super-absorbent resin is given a suitable hydrophilicity to the surface thereof, and the like absorbed urine in the sanitary material can be quickly and widely spread over the surface of the water absorbent resin particles, and as a result, diapers such as sanitary riswet material ( rewet the like) properties and leakage suppression characteristics can significantly be improved. Diffusion characteristics, such as such urine can be confirmed by the embodiment Spreading properties, which will be described later, this Spreading Properties after Lin and uniformly to have a constant thickness and width of the water-absorbent resin lg to 200mm length spread, coming from the dye mixture of 9 parts by weight % time and the physiological saline absorption sikyeoteul 2g is injected at the center of where to lean putting the water-absorbent resin, can be measured and calculated by the maximum length (mm) that the saline solution and to be diffused in the water-absorbent resin. One embodiment the superabsorbent resin is the Spreading and characteristics can be 140 to 200mm, or 145 to 180mm, This allows, it is possible to greatly improve the hygiene material rihet characteristics.
The superabsorbent resin On the other hand, satisfy the various properties example described above one embodiment, after obtaining the hydrogel polymer by the crosslinking polymerization to form a and was dried, pulverized, and classified to a base resin powder, and a surface crosslinking step in the presence of a particular surface cross-linking agent It can be produced by a production method comprising a.
According to another embodiment of the invention, there is provided a method of manufacturing the above-mentioned super-absorbent resin. This manufacturing method comprises the steps of in the presence of an internal crosslinking agent, to form a hydrogel polymer comprising a first cross-linked polymer by cross-linking polymerization of the water-soluble ethylenically unsaturated monomer having at least partially neutralized acid; Forming a function of the gel polymer dried, pulverized and classified to a base resin powder; And in the presence of a surface crosslinking agent, may comprise a step of surface crosslinking by heating a base resin powder, the surface cross-linking agent are common include the compounds, and the common compounds of cyclic alkylene carbonate in a plurality of types are hydrogen bond component the Hansen solubility parameters according to the may be equal to or higher than 13.
Hereinafter, the production method in detail for each step.
First, different implementations of the manufacturing method includes forming a hydrogel polymer by cross-linking polymerization. Specifically, the monomer to the composition in the presence of an internal cross-linking agent comprises a water-soluble ethylenically unsaturated monomer and a polymerization initiator, a thermal polymerization or photo-polymerization to form a hydrogel polymer.
Water-soluble ethylenic unsaturated monomer contained in the monomer composition are as previously described.
In addition, the commercial monomer composition, the polymerization initiator typically used for the production of super-absorbent resin " may be included. Non-limiting examples of the polymerization initiator include thermal polymerization initiator or a photopolymerization initiator may be used in accordance with the polymerization method. However, even in light of the polymerization process, it occurs a certain amount of heat due to ultraviolet radiation, and also a certain amount of heat generated with the progress of the polymerization heat banung banung, may be included to add a thermal polymerization initiation agent.
Here, the photopolymerization initiator is, for example, benzoin ethers (benzoin ether), dialkyl acetophenones (dialkyl acetophenone), hydroxyl-alkyl ketones (hydroxyl alkylketone), phenyl glyoxylic rate (phenyl glyoxylate), benzyl dimethyl ketal (Benzyl Dimethyl ketal), acylphosphine (acyl phosphine) and alpha-wherein the at least one compound selected from the group consisting of amino-ketone (a-aminoketone) may be used. Specific examples of the acylphosphine of that, commercial lucirin TPO, i.e., 2,4,6-trimethyl-to-benzoyl-trimethyl-phosphine oxide may be used (2,4,6-trimethyl-benzoyl-trimethyl phosphine oxide) . For a more variety of photopolymerization initiator
Reinhold Schwalm book is: are disclosed in page 115 of "UV Coatings Basics, Recent Developments and New Application (Elsevier 2007 year)," and you can see it.
In addition, the thermal polymerization initiator include a persulfate-based initiator, an azo type disclosed can be used at least one compound selected from the group consisting of low-1, hydrogen peroxide and ascorbic acid. Specifically, the persulfate-based initiator and sodium sulfate (Sodium persulfate; Na 2 S 2 0 8 ), potassium persulfate (Potassium persulfate; K 2 S 2 0 8 ), ammonium persulfate (Ammonium persulfate; (NH 4 ) 2 s 2 0 8 are exemplified, and so on). Further, azo (Azo) based initiators include 2,2-azobis (2-amidinopropane) dihydrochloride (2,2-azobis (2-amidinopropane) dihydrochloride), 2, 2 _ azobis- (Ν, Ν- dimethylene) isobutoxy Thira Mai Dean dihydrochloride (2,2-azobis- (N, N -dimethylene) isobutyramidine dihydrochloride), 2- ( carbamoyl-azo) isobutyronitrile (2- (carbamoylazo) isobutylonitril), 2,2-azobis [2-Ο imidazolin- 2-Yl) propane] dihydrochloride ( 2 , 2 -azobis [ 2 - ( 2 -imidazolin- 2 -yl) propane] dihydrochloride), 4,4- azobis (4-cyano-ballet rigs acid) (4, 4-azobis- (4-cyanovaleric acid )) the like are exemplified. Than it is disclosed in page 203 of "Principle of Polymerization (Wiley, 1981 year)" which is Odian book for various thermal polymerization initiator, and can refer to it.
The polymerization initiator may be added at a concentration of about 0.001 to 1 parts by weight based on the monomer composition /. That is, when the concentration of the polymerization initiator is too low and may slow the rate of polymerization is not preferable because it can be residual monomers are extracted in a large amount in the final product. On the other hand, it is not preferable because the resin properties such as the concentration of the polymerization initiator over the content of the component for the number becomes the polymer chains that make up the network shorter increased at higher pressure that water absorption capacity is reduced can be lowered.
On the other hand, the monomer composition includes a cross-linking agent ( "internal crosslinking agent") to improve the physical properties of the composition according to the polymerization of the water-soluble ethylenically unsaturated monomer. The cross-linking agent as for the internal cross-linked hydrogel polymer, can be used separately from the "surface cross-linking agent" to be described later.
In particular, in the method for producing another embodiment, the previously described internal crosslinking agent, for example, bis (meth) acrylamides having a carbon number of 8 to 12, with 2 to 10 carbon atoms
Be used as the poly (meth) acrylates having 2 or a poly (meth) allyl ether of a polyol of the polyol to 10, and may This allows to obtain a cross-linked hydrogel polymer is combined inside a properly assigned. However, with regard to the type of internal cross-linking agent, because the previously described bar, additional description thereof will be omitted.
In addition, these internal crosslinking agents may be in an amount of 0.4 part by weight to 2 parts by weight, or from 0.4 to 1.8 parts by weight based on 100 parts by weight of a monomer composition including the internal crosslinking agent and monomer. This allows, may be the optimization function it is to break the polymer and the internal degree of crosslinking of the base resin powder control, and the ability to absorb liquid and the whole of the water-absorbent resin. However, the larger the amount of the internal cross-linking agent is too, can be a basic absorption performance of the super-absorbent resin decreases.
In addition, the monomer composition has an additive such as a thickener, a plasticizer, a preservation stabilizer, an antioxidant can be further included if necessary.
Then, this monomer composition can be a raw material such as the above-described monomer, a polymerization initiator, an internal crosslinking agent prepared in the form of a solution dissolved in a solvent.
At this time, a usable solvent as long as it can dissolve the above-described raw materials may be used without any limitation in its configuration. For example, the solvents include water, ethanol, ethylene glycol, diethylene glycol, triethylene glycol, 1,4-butane dieul, propylene glycol, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, methyl ethyl ketone, acetone, methyl amyl ketone, cyclo hex rice, cyclopentanone, diethylene glycol monomethyl ether, diethylene glycol ethyl ether, a lactone of a toluene, xylene, butynyl, carboxylic ratio, a methyl cells cellosolve acetate, etc. may be used, Ν, Ν- dimethylacetamide, or a common compound.
And, forming a hydrogel polymer by polymerization of the monomer composition can be carried out in a conventional polymerization process, the process is not particularly limited. Non-limiting examples, the polymerization method I significantly nadwi as thermal polymerization and photo polymerization according to the type of the polymerization energy source, if the progress of the thermal polymerization can be conducted in a reactor having an axis agitation, such as a kneader (kneader), light when proceeding the polymerization it may take place in a half unggi provided with a movable conveyor belt.
For example, by putting the monomer composition in the reactor such as a kneader equipped with a stirring shaft, and a thermal polymerization by supplying hot air to this heating, the reactor or can be obtained hydrogel polymer. In this case, the function to be discharged to the discharge port depending on the type of anti-unggi stirring shaft provided with a half unggi polymer gel can be obtained particles of a few millimeters to several centimeters. Specifically, the hydrogel polymer is obtained may be obtained in various forms depending on the concentration and the injection rate of the monomer composition to be injected, it is normal (weight average) grain size of 2 to 50 mm hydrogel polymer can be obtained. And, one another example, if the progress of photopolymerization of the monomer composition in the movable half unggi provided with a conveyor belt has a hydrogel polymer in the form of a sheet can be obtained. That case that there the thickness of the sheet may vary depending on the concentration and the injection rate of the monomer composition to be injected, to ensure the production speed, but that the entire sheet can be uniformly polymerized, usually adjusted to a thickness of 0.5 to 10 cm desirable.
The normal water content of the hydrogel polymer obtained in the same method may be 40 to 80% by weight. On the other hand, in the present specification, "water content" means a value in the weight of the hydrogel polymer in an amount of water which accounts for the entire hydrogel polymer weight minus the weight of the dry polymer. Specifically, by measuring the weight decrease due to evaporation of water in the polymer in the course of heating up through infrared drying the temperature of the polymer is defined as a calculated value. At this time, the drying conditions were a total drying time in such a manner as to keep the back in a 180 ° C raising the temperature from room temperature to 18CTC is set to 20 minutes, including 5 at a temperature ramping up step, to measure the water content.
Next, the function carried out, thereby obtaining the step of drying the polymer gel. If necessary may be further subjected to a step that reference the hydrogel polymer before drying to increase the efficiency of the drying stage grinding.
At this time, the crusher to be used is limited to the configuration, but, specifically, a vertical cutter (Vertical pulverizer), turbo cutter (Turbo cutter), a turbo grinder (Turbo grinder), rotary cutting mill (Rotary cutter mill), cutting mill (cutter mill), disc mill (disc mill), a piece crusher (Shred crusher), crusher (crusher), the chopper (chopper) and one-plate type cutting machine including any one selected from the grinding machine the group consisting of (disc cutter) It can be, but is not limited to the above example.
The pulverized step may be crushed into a grain size of 2 to 10mm in the hydrogel polymer. The particle size is milled to less than 2 mm is not easy technically because of the high water content of the hydrogel polymer, and may also appear to be ungjip each other between the ground particles developing. On the other hand, if the particle size is milled to 10 mm, greater than it may be minimal increase the efficiency effect of the drying step further comprises.
Or pulverized as described above or carries out a drying for a hydrogel polymer immediately after the polymerization step without passing through the pulverized. The drying temperature of the drying is 150 to 250 ° may be C. The drying temperature is 150 ° is less than C, and that the drying time is too longer and formed end is a fear that the physical properties of the water absorbent resin decreases, and the dry silver is 250 ° when it exceeds C, the drying only over the polymer surface, comprising further may result in a differential in the milling process, there is a high possibility that the physical properties of the water absorbent resin reduced to be finally formed. Therefore, preferably the drying is 150 to 200 ° will be at a temperature of C, more preferably 170 to 195 ° can be carried out at a temperature of C.
On the other hand, when the drying time, in consideration of process efficiency, but to proceed for 20 to 90 minutes, but is not limited to this.
The drying method of the drying step as long as it is also commonly used in the drying step of the hydrogel polymer may be used are selected, without limitation of its construction. Specifically : it may be carried out a drying step, for example by supplying hot air, infrared irradiation, microwave irradiation, or UV irradiation. The water content after the drying phase, such a polymer may be from about 0.1 to about 10% by weight.
Next, the steps of crushing the dried polymer obtained through this drying steps.
After the grinding step the resulting polymer powder may be a particle diameter of 150 to 850 m. The mill which particle size is used to crush the same specifically, pin mill (pin mill), a hammer mill (hammer mill), screw mill (screw mill), a mill (roll mill), disc mill (disc mill) or the jog but you can use a mill (jog mill) or the like, not limited to the above example.
And, in order to manage these physical properties of the super-absorbent resin powder after the final commercialization of the milling step, depending on the particle size of the polymer powder obtained after grinding
It may be subjected to a separate process of classification. Preferably the particle size is classified to the polymer 150 to 850 zm, can be commercialized after the surface cross-linking step banung only polymer powder having such a particle size. As for the particle size distribution of the base resin powder obtained by this process, so a bar previously described, no further detailed description thereof will be omitted.
On the other hand, after the manufacture of the base resin powder through to the above-described classifying process it can be high in the presence of a surface crosslinking agent, and heat-treating the base resin powder surface crosslinking the water absorbent resin particles. The surface cross-linking are the surface cross-linked layer on the surface of the base resin particles to induce cross-linking banung on the surface of the base resin powder in the presence of a surface cross-linking agent, with such a surface cross-linking can be formed.
In more detail, the above-described different implementations of the manufacturing method, including a common compound of the plural kinds of cyclic alkylene carbonate in and, there is used a surface cross-linking agent having a Hansen solubility parameter of 13 yisangwa hydrogen bonding component, such a surface cross-linking agent as for the kind of the same, so already discussed fully above, further description thereof will be omitted.
In the surface cross-linking step with the surface cross-linking agent, the amount of the surface cross-linking agent may be appropriately adjusted depending on the specific type or banung conditions of the crosslinking agent, and preferably be adjusted as part of 0.001 to 5 parts by weight per 100 parts by weight of the base resin powder can. When the too low amount of the surface cross-linking agent, a surface modification can not be achieved properly, the physical properties of the final resin can be lowered. Conversely an excess of the surface crosslinking agent is used because of the excessive surface cross-linking banung is not preferred because the absorption capacity of the basic resin can be even reduced. Eu
On the other hand, the surface cross-linking agent there is added to the base resin powder in the surface cross-linked liquid state comprising the same, as for the method of addition of the surface cross-linking solution there is no particular limitation in its configuration. For example, the surface cross-linked into a liquid and a base resin powder article banung heunhap or base method of the resin surface crosslinking aekreul spraying a powder, it was continuously supplied to a base resin powder and the surface cross-linking solution in the mixer being continuously driving a common summing You can use the methods.
In addition, the surface cross-linking solution may further include water and / or hydrophilic organic solvent as a medium. This allows, such as surface cross-linking agent has the advantage that can be uniformly dispersed in the base resin powder. At this time, the water and the content is picked dissolved / induce the dispersion and the base resin powder agglomeration phenomenon prevention, and at the same time 100 base resin powder for the purpose of optimizing the surface depth of penetration of the surface cross-linking agent for the parts by weight of a surface crosslinking agent of the hydrophilic organic solvent for it can be applied by adjusting the addition rate. The surface cross-linking solution is added to a base resin powder 14CTC to 200 for ° C, graphite is 170 ° C to 195 ° 5 to 60 minutes in the reaction up to a temperature of C, or 10 minutes to 50 minutes, or 20 minutes to 45 minutes may be carried out a surface crosslinking banung. More specifically, the surface cross-linking step is 20 ° C to 130 ° C, graphite is 40 ° C to about 120 ° and the temperature was raised to from the initial temperature of the C 10 min or more, or the maximum temperature of the banung over a period of 10 minutes to 30 minutes , it may be done by heat treatment to keep the maximum temperature for 5 minutes to 60 minutes.
These surface cross-linking process condition suitably layer of physical properties such as more excellent liquid cylinder by a meeting (in particular, banung conditions at elevated temperature conditions and banung highest temperature) , the group " a super-absorbent resin can be produced.
Temperature raising means for the surface cross-linking reaction is not particularly limited. Supplying a heating medium, or can be heated to supply the heat source directly. At this time, as a type of available heating medium, but can use a fluid such as an elevated temperature, such as steam, hot air, hot oil, not limited to this, and the temperature of the heating medium to be supplied is the means, the rate of rise and temperature rise target temperature of the heating medium It can be appropriately selected in consideration. On the other hand, as a heat source is directly supplied to the heating by electricity, but include a method of heating with a gas, it is not limited to the above example.
The super-absorbent resin obtained by the above manufacturing method is greatly improved and the like the ability to absorb and barrel while being liquid and so on are maintained excellently, it can be spread widely and the like absorbed urine in the sanitary material, sanitary material riswet characteristics, such as beam SAT can.
【Effects of the Invention】
Super-absorbent resin according to the present invention, a basic absorbent such as performance and barrel-component such as a solid, yet can be maintained, the absorbent material in the sanitary urine superabsorbent resin
. It can be quickly and widely spread along the surface of the particles. As a result, the super-absorbent resin of the present invention it is possible to improve the hygiene material riswet (rewet) suppressing properties and leakage properties.
[Mode for Carrying out the invention]
Hereinafter, the preferred embodiments are set forth to aid the understanding of the invention but eu following examples are only intended to illustrate the invention only, and are not intended to limit the invention to these.
Example 1
Acrylic acid 500 g, polyethylene glycol diacrylate (Mw = 52 was dissolved by the addition of phosphine oxide O.Olg - 3), 3 g of common after combined, diphenyl (2,4,6-trimethylbenzoyl) was added. Then, the aqueous solution of the water-soluble unsaturated monomer and the added nitrogen is continuously added to 896.4g of aqueous solution of sodium hydroxide and 24.5% by weight was prepared. Next, the classifying the temperature of the aqueous solution of 5 (and nyaenggak a C, to ultraviolet light in an aqueous solution irradiated 90 seconds to obtain a polymer functions gel. The obtained function, the gel polymer was ground using a grinder. Sieve standard network of the ASTM standard 150 / a base resin powder were prepared having a particle diameter of ΛΠ to 850 // m.
Then, the, glyceryl for the prepared base resin powder 100 parts by weight of carbonate (Hansen solubility parameters according to the hydrogen bond component: 18.9) 1 part by weight of propylene carbonate (Hansen solubility parameter of hydrogen bonding seokbun: 10.8) 1 part by weight, and water 4 parts by weight of the combined portions common to prepare a surface cross-linking solution eu this surface cross-linking in the liquid, the glyceryl based on the respective solubility parameter of the carbonate and propylene carbonate, one hydrogen of the surface cross-linking agent of the common compounds status calculation thereof, the weight average value Hansen solubility parameters according to the binder component was calculated as 14.85. For reference, the solubility parameter is a value measured by the common only to compound the weight average value of the surface cross-linking of the liquid except the water, glyceryl carbonate, and propylene carbonate.
Then, the injection liquid in the surface cross-linked base resin powder and the mixture was stirred at room temperature was heunhap to the surface cross-linking solution evenly distributed in the base resin powder. Then, into a base resin powder heunhap the surface cross-linking solution on the surface cross-linking reactor and proceed to the surface cross-linked banung. Within this surface cross-linking reactor, a base resin powder is 80 ° 190 later was found to be gradually raised from the initial temperature in the vicinity of C, 30 minutes, ° was operated to reach a maximum temperature of banung C. After reaching such maximum temperature banung, it was added for 30 minutes and taken banung the superabsorbent polymer sample the final manufacturing. Embodiment having the above surface cross-linking step and then, the particle diameter of 150 m to 850 m by classifying sieve of standard mesh ASTM standard was prepared in the super-absorbent resin of Example 1.
Example 2
A base resin powder was prepared in the same manner as in Example 1.
Surface cross-linking solution for the manufacture of, 100 parts by weight of the base resin powder, glycerol carbonate (Hansen solubility parameters according to the hydrogen bond component: 18.9) 1.5 parts by weight of propylene carbonate (Hansen solubility parameters according to the hydrogen bond component: 10.8) 0.9 parts by weight and the surface cross-linking solution was prepared 4 parts by weight of water were combined common. In such a surface cross-linking solution, Hansen solubility parameters according to the hydrogen bond component of the glyceryl carbonate and propylene respective solubility relative to the parameters, the surface cross-linking agent of the common compounds conditions calculated to counter the weight average value of the polycarbonate was calculated as 15.86. For reference, the solubility parameter Ada the exception of water of the surface cross-linking solution, and measuring the weight of glyceride with an average value. Only traces of compound carbonate and propylene carbonate value.
The process proceeds to later in Example 1, and the surface cross-linking, such as the same method to prepare a super-absorbent resin of Example 2 having a particle diameter of 1 to 150 850.
Example 3
A base resin powder was prepared in the same manner as in Example 1.
For surface cross-linking solution prepared when 100 parts by weight of the base resin powder, glyceryl carbonate (Hansen solubility parameters according to the hydrogen bond component: 18.9) 1 part by weight ethylene carbonate (Hansen solubility parameters according to the hydrogen bond component: 12.3) 1 part by weight the combined common part and the water 4 parts by weight to prepare a surface cross-linking solution. Hansen solubility parameters according to such a surface cross-linking in a liquid, the glyceryl based on the respective solubility parameter of the carbonate and ethylene carbonate, by weight of this hydrogen bond component of the surface cross-linking agent of the common state compound calculated as the average value was calculated as 15.6- . For reference, the solubility parameter is a value measured by the common only to compound the weight average value of the surface cross-linking of the liquid and, glyceryl carbonate, ethylene carbonate, and, except for water.
Thereafter, the exemplary process proceeds deungol For surface cross-linking in one and the same way to prepare a super-absorbent resin of Example 3 having a particle diameter of 150 to.
Example 4
A base resin powder was prepared in the same manner as in Example 1.
For surface cross-linking solution prepared when 100 parts by weight of the base resin powder, glyceryl carbonate (Hansen solubility parameters according to the hydrogen bond component: 18.9) 1 part by weight ethylene carbonate (Hansen solubility parameters according to the hydrogen bond component: 12.3) 0.5 the combined common part and the water 4 parts by weight to prepare a surface cross-linking solution. In such a surface cross-linking solution, Hansen solubility parameters according to the hydrogen bond component of the glycerol carbonate and the ethylene compound while the common relative to the respective solubility parameter, calculated as the weight thereof, the average value of the carbonate surface cross-linking agent was calculated as 16.7. For reference, the solubility parameter is a value measured by the common only to compound the weight average value of the surface cross-linking of the liquid and, glyceryl carbonate, ethylene carbonate, and, except for water.
The process proceeds to later in Example 1, and the surface cross-linking, such as the same method to prepare a super-absorbent resin of Example 4 having a particle size of 150 to 850 皿 1.
Comparative Example 1
A base resin powder was prepared in the same manner as in Example 1.
Surface cross-linking solution for the manufacture of, 100 parts by weight of the base resin powder, ethylene carbonate (Hansen solubility parameters according to the hydrogen bond component: 12.3) 1.0 parts by weight of propylene carbonate (Hansen solubility parameters according to the hydrogen bond component: 10.8) 1.0 parts by weight and the surface cross-linking solution was prepared 4 parts by weight of water were combined common. In such a surface cross-linking solution, Hansen solubility parameters according to the hydrogen bond component of the ethylene carbonate and propylene carbonate, based on the respective solubility parameter, of the common state compound calculated as a weight average value thereof, the surface cross-linking agent was calculated as 11.55. For reference, the solubility parameter is a except for water of the surface cross-linking solution, an ethylene carbonate and a measurement only by the weight-average values in common compound of propylene carbonate value.
The process proceeds to later in Example 1, and the surface cross-linking, such as the same method to prepare a super-absorbent resin of Comparative Example 1 having a particle size of 150 m to 850 / im.
Comparative Example 2
A base resin powder was prepared in the same manner as in Example 1.
Surface cross-linking solution for the manufacture of, 100 parts by weight of the base resin powder, ethylene carbonate (Hansen solubility parameters according to the hydrogen bond component: 12.3) 1.0 parts by weight of the combined common and 4 parts by weight of water to prepare a surface cross-linking solution. In such a surface cross-linking solution, Hansen solubility parameters according to the hydrogen bond component of the ethylene carbonate, the surface cross-linking agent, relative to the baseline of the solubility parameter, calculated as the average value of the weight thereof is 12.3 in. For reference, the solubility parameter is a value that, except for water of the surface cross-linking solution, and measuring the weight average value only for the ethylene carbonate.
Since the same procedures as in Example 1, the process proceeds to such a surface cross-linking, 150 // prepare a super-absorbent resin of Comparative Example 2 having a particle size of m to 850 / im.
Comparative Example 3
A base resin powder was prepared in the same manner as in Example 1.
For surface cross-linking solution prepared when 100 parts by weight of the base resin powder, glyceryl carbonate (Hansen solubility parameters according to the hydrogen bond component: 18.9) 1.5 parts by weight of the combined common and 4 parts by weight of water to prepare a surface cross-linking solution. In such a surface cross-linking solution, Hansen solubility parameters according to the hydrogen bond component of the glyceride relative to the solubility parameter of the carbonate, calculated as weight average value thereof, the surface crosslinking agent is 18.9. For reference, the solubility parameter is a value that, except for water of the surface cross-linking solution, and measuring the weight average value only in the glyceryl carbonate.
Then, the process proceeds to the surface cross-linked, such as in the same manner as in Example 1, to prepare a super-absorbent resin of Comparative Example 3 having a particle diameter of 150 to 850 / zm.
Comparative Example 4
A base resin powder was prepared in the same manner as in Example 1.
Surface cross-linking solution prepared when, based on 100 parts by weight of a base resin powder, propylene carbonate was prepared the (Hansen solubility parameters according to the hydrogen bond component 10.8) 1.5 parts by weight of water and 4 parts by weight of common surface cross-linked liquid portions were combined. In such a surface cross-linking solution, Hansen solubility parameters according to the hydrogen bond component of the propylene carbonate the surface cross-linking agent, relative to the baseline of the solubility parameter, calculated as the average value of the weight thereof is 10.8. For reference, the solubility parameter is a value that, except for water of the surface cross-linking solution, and measuring the weight average value only for the propylene carbonate.
The process proceeds to later in Example 1, and the surface cross-linking, such as the same method to prepare a super-absorbent resin of Comparative Example 4 having a particle size of 150 to 850 rni.
Experimental Example
Subjected to a physical property of each super-absorbent resin prepared in Examples and Comparative Examples were measured and evaluated in the following manner.
(1) particle size evaluation
Embodiment and the diameter of the base resin powder and a super-absorbent resin used in Comparative Examples were measured according to the European Nonwoven Industry Association (European Disposables and Nonwovens Association, EDANA) standard ED ANA method WSP 220.3.
(2) centrifuging beam SAT (CRC, Centrifuge Retention Capacity)
European nonwovens industry association (applicable European ' a Disposables and Nonwovens Association, EDANA) standard centrifugation Bo SAT (CRC) by Mucha Heavy absorption magnification measured according to EDANA WSP 241.3. Superabsorbent Polymer W 0 (g, about 0.2g) after the insert uniformly in the envelope of the nonwoven fabric is sealed (seal), 0.9 parts by weight of room temperature 0 / 0 were submerged in saline solution of sodium chloride solution. After 30 minutes using a centrifuge after the envelope, leave for 3 minutes to dry 250G weight W of the bag 2 were measured in (g). Further, after the same operation and without using the water-absorbent resin were measured by mass W! (G) at that time. In this way use of the respective mass obtained by the following equation 1 to calculate the CRC (g / g)
Beam SAT was OK.
[Equation 1]
CRC(g/g) = {[W2(g) - W!(g) - Wo(g)]/W0(g)}
(3) a gel bed permeability (GBP, Gel Bed Permeability)
A free swell gel bed permeability (GBP) of the physiological saline was measured according to the following method described in Korea patent application No. I 110-2014-7018005.
Specifically, the Korea was used the apparatus shown in the drawings Patent Application No. 10-2014-7018005 to measure the Free Swell GBP. First, add the device to position the plunger in the empty sample vessel and measuring the height of the using a suitable gauge accuracy 0.01 mm, up to the sample container from the upper portion of the weight floor. During measurement, force applied to the thickness gauge was adjusted to less than about 0.74 N. On the other hand, the US standard 30 mesh screen of the super-absorbent resin to be measured is passed, and the GBP, US standard 50 mesh screened superabsorbent polymer is maintained above the screen by a particle size of 300 to 600 and to obtain a water-absorbent resin.
Thus, insert the super-absorbent resin of the classified 2.0 g of the sample in the container, spread evenly over the bottom of the sample vessel. Then, the high-soaked for about 60 minutes under no pressure in the container does not contain more state with the plunger in 0.9% saline was swell the water-absorbent resin. In this case, it was used as the sample containers which do not affect the movement of the physiological saline was put into a liquid so that some of the storage up than the bottom looking up the sample container on a mesh located in the liquid reservoir, wherein the mesh roneun sample container. The surface in the sample vessel while the height of the saline solution is saturated was adjusted to defined by the superabsorbent polymer swelling rather than saline.
At the end of this period, place the assembly of the plunger and the weight mounted on the swollen superabsorbent polymer in the sample container, and then taken out the sample container, the plunger, the weight and the swollen superabsorbent polymer from the solution. Then, before measuring GBP, sample container, the plunger, the weight and the swollen water-absorbent resin and the flat and of uniform thickness of a large grid non-deformable plate was placed on it for about 30 seconds. Then, by using the same thickness gauge that was used earlier, was re-measuring the height of the bottom of the sample container from the top of the weight. Then, the above additional devices the plunger to empty the samples swell the height measured values of that device located within the container and to the in height measured values of the unit containing the water-absorbent resin thickness of the black of the swollen superabsorbent polymer has a height 'Ή " It was obtained.
For GBP measurements, swelling of superabsorbent resin, and a plunger was added containing flow coming from a 9% by weight of normal saline in a sample container. Normal saline were adjusted so that the flow rate of the saline solution into the sample vessel (flow rate) is consistent head pressure equal to the height of the sample container shown to ensure that an overflow into the top of the cylinder. Then, by using the scale and beaker, the amount versus time of the solution passing through the swollen super-absorbent resin were measured by the weight measurement method. Once the overflow begins, the data points were collected from balance every second for at least 60 seconds. Flow rate of the swelling and through the water-absorbent resin (Q) is, in g / sec basis by the swelling and linear least-square fit of fluid (g) vs. time (sec) passing through the water-absorbent resin (linear least-square fit) It was determined.
This value was calculated using the obtained data the GBP (citf) by the following equation 2.
[Formula 2]
R = [(^ x H x M] / [D x p x P]
In the above formula 3, K is a gel . Bed permeability (cuf) and, Q is the flow rate (g / sec), and, H is the swelling and the height (cm) of the water absorbent resin, μ is about lcP viscosity of the saline solution used for the liquid viscosity (Ρ) (this test ), and, a is the cross-sectional area (for the sample containers used for this test 28.27oif) and, p is the liquid density (g / crf) (about 1 g / cirf for the physiological saline used for this test) for the liquid flow, P is the hydrostatic pressure (dyne / an 2 ) (normally approximately 7,797 dyne / cin 2 a). Hydrostatic pressure is formula P = ρ χ g χ is calculated from h, where p is the liquid density (g / cirf) and, g is the gravity acceleration (nominally in the 981 cm / sec 2 a), h is a filling height (e.g. g., a 7.95 cm) for the GBP test described herein.
Testing the at least two samples, and as a result the average to high conversion to determine the Free Swell GBP of the water-absorbent resin, and a unit darcy (1 darcy = 0.98692 x 10 8 was cuf).
(4) Spreading properties (mm)
Examples and Comparative Examples and the water absorbent resin uniform thickness lg to 200mm length, and
After uniformly spreading lean to have a width, when and the dye is mixed with 0.9 weight% physiological saline 2g sikyeoteul absorbed by the water absorbent resin injected into the center of the spread Lin place, up to which the physiological saline solution and to be diffused in the water-absorbent resin in length ( It was measured and calculated in mm)
The embodiment with the above measuring method in Example 1
To the value shown in Table 1 collectively.
TABLE 1
Referring to Table 1, Examples 1 to 4 is a basic absorption performance (CRC) Comparative Example 1 while equally appeared at a level above and to 4, barrel-component (GBP) and to Spreading properties are significantly superior to the Comparative Example Urine It was found to be widely spread and so on.
Claims
Water-soluble ethylenic base resin including a first cross-linked polymer of an unsaturated monomer having a powder at least partially neutralizing the acid; And
A super-absorbent resin which is formed on the base resin. Powder, and wherein the first crosslinked polymer comprises a cross-linked surface layer and a second cross-linked polymer cross-linking the surface cross-linking agent is added to the medium,
The surface cross-linking agent comprises a common compound of cyclic alkylene carbonate in a plurality of types, and wherein the compound is a common super-absorbent resin having a Hansen solubility parameters (Hansen solubility parameter) by the hydrogen-bonding component (hydrogen bonding component) 13
[Claim 2]
The method of claim 1, wherein the Hansen solubility parameter and the water absorbent resin is calculated as a weight average value of the parameter value of each cyclic alkylene carbonate contained in the common compounds according to the hydrogen bond component.
[Claim 3]
The method of claim 1, wherein the common compounds are Hansen solubility parameter of between 10 and 13, the first and the cyclic alkylene carbonate, the Hansen solubility parameters according to the hydrogen bond component 16 to 20 of the second ring by the hydrogen bond component super-absorbent resin containing a type alkylene carbonate.
[Claim 4]
The method of claim 3 wherein the super-absorbent resin to the first cyclic alkylene carbonate comprises ethylene carbonate or propylene carbonate, and the second cyclic alkylene carbonate comprises a glyceryl carbonate.
[5.]
4. The method of claim 3 wherein the first and second cyclic alkylene carbonate is 0.9: super-absorbent resin contained in a weight ratio of 2: 1 to 1.
[6.]
The method of claim 1 wherein the superabsorbent polymer is 27g / g to 37g / g of centrifuged beam represents the SAT (CRC), and represents the gel bed permeability (GBP) of 23 to 35darcy absorbing resin.
[7.]
In the presence of an internal crosslinking agent, to form a hydrogel polymer comprising a first cross-linked polymer by polymerizing a water-soluble cross-linked ethylenically unsaturated monomer having at least partially neutralized acid;
Forming a function of the gel polymer dried, pulverized and classified to a base resin powder; And
In the presence of a surface cross-linking agent, and including the step of surface crosslinking by heating a base resin powder,
The surface cross-linking agent comprises a common compound of cyclic alkylene carbonate in a plurality of types, and wherein the common compound is the hydrogen bonding component (hydrogen bonding component) Hansen solubility parameters (Hansen solubility parameter) of 13 or more to claim 1. super-absorbent composition according to the the method of manufacture.
[8.]
The method of claim 7, wherein the water-soluble ethylenically unsaturated monomer is acrylic acid, methacrylic acid, maleic anhydride, fumaric acid, crotonic acid, itaconic acid, ethanesulfonic acid one by one ethanesulfonic acid, 2-methacryloyloxyethyl 2-acrylic, 2- (meth) acid, or 2- (meth) acrylamide-2-methyl anionic monomers and their salts of the sulfonic acid with an acrylic; (Meth) acrylamide, N- substituted (meth) acrylate, 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, methoxy polyethylene glycol, hydroxyethyl (meth) acrylate or polyethylene
Glycol (meth) non-ionic hydrophilic monomers containing acrylate; And (Ν, Ν)-dimethylaminopropyl (meth) an amino group-containing unsaturated monomer of acrylamide and their quaternary cargo-dimethylaminoethyl (meth) acrylate or (Ν, Ν); at least one selected from the group consisting of method for producing a superabsorbent resin comprising.
[9.]
The method of claim 7, wherein the internal cross-linking agent include poly (meth) of the poly (meth) acrylate and a polyol having 2 to 10 carbon atoms of a carbon number of 8-bis (meth) acrylamide to 12, 2 to 10 carbon atoms polyol. Allyl ether and process for producing a water absorbent resin containing at least one selected from the group consisting of.
[10.]
The method of claim 7, wherein the base resin powder A method of manufacturing a super-absorbent resin to be pulverized and classified to have a particle diameter of 150 to 850 1.
[Claim 111
The method of claim 7, wherein the surface cross-linking step is 20 ° C to 130 ° C 140 over a period of 10 minutes to 30 minutes at an initial temperature in ° C to 200 ° and the temperature was raised to a maximum temperature of C, to 5 minutes for the highest temperature for 60 minutes to process for producing a superabsorbent polymer which is conducted by the heat treatment.
| # | Name | Date |
|---|---|---|
| 1 | 201917016686-TRANSLATIOIN OF PRIOIRTY DOCUMENTS ETC. [26-04-2019(online)].pdf | 2019-04-26 |
| 2 | 201917016686-STATEMENT OF UNDERTAKING (FORM 3) [26-04-2019(online)].pdf | 2019-04-26 |
| 3 | 201917016686-PROOF OF RIGHT [26-04-2019(online)].pdf | 2019-04-26 |
| 4 | 201917016686-PRIORITY DOCUMENTS [26-04-2019(online)].pdf | 2019-04-26 |
| 5 | 201917016686-FORM 1 [26-04-2019(online)].pdf | 2019-04-26 |
| 6 | 201917016686-DECLARATION OF INVENTORSHIP (FORM 5) [26-04-2019(online)].pdf | 2019-04-26 |
| 7 | 201917016686-COMPLETE SPECIFICATION [26-04-2019(online)].pdf | 2019-04-26 |
| 8 | 201917016686.pdf | 2019-05-16 |
| 9 | 201917016686-OTHERS-010519.pdf | 2019-05-20 |
| 10 | 201917016686-Correspondence-010519.pdf | 2019-05-20 |
| 11 | 201917016686-FORM-26 [10-06-2019(online)].pdf | 2019-06-10 |
| 12 | 201917016686-Power of Attorney-110619.pdf | 2019-06-19 |
| 13 | 201917016686-Correspondence-110619.pdf | 2019-06-19 |
| 14 | 201917016686-FORM 3 [04-10-2019(online)].pdf | 2019-10-04 |
| 15 | 201917016686-FORM 18 [03-05-2021(online)].pdf | 2021-05-03 |
| 16 | 201917016686-FER.pdf | 2021-10-18 |
| 17 | 201917016686-OTHERS [01-11-2021(online)].pdf | 2021-11-01 |
| 18 | 201917016686-FER_SER_REPLY [01-11-2021(online)].pdf | 2021-11-01 |
| 19 | 201917016686-CLAIMS [01-11-2021(online)].pdf | 2021-11-01 |
| 20 | 201917016686-ABSTRACT [01-11-2021(online)].pdf | 2021-11-01 |
| 21 | 201917016686-Response to office action [16-02-2022(online)].pdf | 2022-02-16 |
| 22 | 201917016686-PatentCertificate23-08-2022.pdf | 2022-08-23 |
| 23 | 201917016686-IntimationOfGrant23-08-2022.pdf | 2022-08-23 |
| 1 | 2021-05-0714-18-10E_07-05-2021.pdf |