WO2017171208A1 - Résine superabsorbante et son procédé de production - Google Patents

Résine superabsorbante et son procédé de production Download PDF

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Publication number
WO2017171208A1
WO2017171208A1 PCT/KR2017/000054 KR2017000054W WO2017171208A1 WO 2017171208 A1 WO2017171208 A1 WO 2017171208A1 KR 2017000054 W KR2017000054 W KR 2017000054W WO 2017171208 A1 WO2017171208 A1 WO 2017171208A1
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Prior art keywords
meth
polymer
particles
base resin
water
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PCT/KR2017/000054
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English (en)
Korean (ko)
Inventor
이혜민
서성종
윤형기
Original Assignee
주식회사 엘지화학
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Priority claimed from KR1020160063524A external-priority patent/KR101863350B1/ko
Application filed by 주식회사 엘지화학 filed Critical 주식회사 엘지화학
Priority to EP17775633.5A priority Critical patent/EP3336134B1/fr
Priority to CN201780003648.6A priority patent/CN108350188B/zh
Priority to US15/767,903 priority patent/US10988582B2/en
Publication of WO2017171208A1 publication Critical patent/WO2017171208A1/fr

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04Homopolymers or copolymers of esters
    • C08L33/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical

Definitions

  • the present invention relates to a super absorbent polymer and a method for producing the same, which exhibits improved liquid permeability while maintaining good absorption performance.
  • Super Absorbent Polymer is a synthetic polymer material capable of absorbing water of 500 to 1,000 times its own weight.As a developer, super absorbent material (SAM) and absorbent gel (AGM) They are named differently. Such super absorbent polymers have been put into practical use as physiological devices, and are currently used in sanitary products such as paper diapers for children, horticultural soil repair agents, civil engineering, building index materials, seedling sheets, freshness-retaining agents in food distribution, and It is widely used as a material for steaming.
  • these superabsorbent polymers are widely used in the field of sanitary products such as diapers and sanitary napkins.
  • the superabsorbent polymers need to exhibit high absorption of moisture and must not escape moisture absorbed by external pressure.
  • it is necessary to maintain the shape well even in the state where the water is absorbed by volume expansion (swelling) to exhibit excellent permeability.
  • the superabsorbent resin is not limited to the outer layer and has excellent physical properties. In order to maintain shape, it is necessary to have a higher gel strength on its own,
  • the superabsorbent polymer particles need to maintain their shape even after they have absorbed water and swelled to maintain voids between the particles and the particles. This is because the voids between the particles act as flow paths to ensure excellent liquid permeability of the superabsorbent polymer. For this reason, in order to provide the superabsorbent polymer which exhibits the improved fluid permeability and other outstanding physical properties as mentioned above, such a superabsorbent resin needs to exhibit higher gel strength.
  • the present invention includes a base resin powder comprising a first crosslinked polymer of a water-soluble ethylenically unsaturated monomer having at least a portion of neutralized acid groups;
  • Absorbance represented by the following formula 1 is 45 to 65g / g
  • the base resin powder to which the hydrophobic inorganic particle is added is subjected to a surface treatment.
  • a surface treatment comprising the step of crosslinking.
  • a super absorbent polymer according to a specific embodiment of the present invention and a manufacturing method thereof will be described in more detail. However, this is presented as an example of the invention, whereby the scope of the invention is not limited, it is apparent to those skilled in the art that various modifications to the embodiments are possible within the scope of the invention.
  • AUP shows the pressure-absorbing capacity for 1 hour under o.7psi for the physiological saline solution (0.9 weight 0 /. Sodium chloride solution) of the super absorbent polymer
  • the inventors of the present invention continually studied to further improve the liquid permeability of the superabsorbent polymer, and as a result, the conditions of the manufacturing process of the superabsorbent polymer described later .
  • the type and content of the internal crosslinking agent described below and the polymerization conditions are optimized to obtain a base resin powder having a high gel strength, and specific surface crosslinking conditions (for example, two specific inorganic particles are used in sequence, and the surface Preferred cross-linking temperature conditions As the surface crosslinking proceeds under the above), it has been found that a superabsorbent polymer can be provided that exhibits significantly improved liquid permeability than previously known while maintaining excellent absorption performance.
  • the surface cross-linking layer can further increase the gel strength of each of the superabsorbent polymer particles
  • the superabsorbent polymer of one embodiment has a very high gel strength of 9,000 to 18,000 Pa
  • the 70 to 190 ('1 (T 7 cm 3 s / g) can exhibit a significantly improved liquid permeability
  • the super absorbent polymer of one embodiment is the absorption of the 45 to 65g / g, as the internal cross-linked structure and the surface cross-linked structure is optimized It can exhibit a good absorption performance defined by degrees.
  • a base resin powder can be obtained through a process such as drying, pulverization and classification.
  • the superabsorbent polymer obtained is suitably manufactured and provided to have a particle size of 150 to 850 // m, or 150 to 710 zm. More preferably, the base resin powder and has a high, at least 95 weight 0 /. Particle size of more than 150 to 710 ⁇ 1 of the water-absorbent resin obtained therefrom, and 3 is a differential having a particle size of less than 150 parts by weight 0 / less than 0, The black may be less than 1.5 weight 0 /.
  • the super absorbent polymer of the embodiment may more properly exhibit the above-described physical properties.
  • alkylene carbonate having 2 to 5 carbon atoms that can be used as the surface crosslinking agent include ethylene carbonate, propylene carbonate, butylene carbonate, and the like. to be.
  • the method of preparing the superabsorbent polymer may include forming a hydrogel polymer including a first crosslinked polymer by thermally polymerizing or photopolymerizing a monomer composition including a water-soluble ethylenically unsaturated monomer, an internal crosslinking agent, and a polymerization initiator; Drying the hydrogel polymer; Grinding and classifying the dried polymer to form a base resin powder; And treating the hydrophobic inorganic particles with respect to the base resin powder, and performing surface crosslinking using the surface crosslinking liquid including the hydrophilic inorganic particles and the surface crosslinking agent described above.
  • the said polymerization initiator will not be specifically limited if it is generally used for manufacture of a super absorbent polymer.
  • the photopolymerization initiator may be used without any limitation as long as it is a compound capable of forming radicals by light such as ultraviolet rays.
  • photopolymerization initiator examples include benzoin ether, dialkyl acetophenone, hydroxyl alkylketone, phenyl glyoxylate, and benzyl dimethyl ketal. Ketal), acyl phosphine and alpha-aminoketone can be used at least one selected from the group consisting of.
  • acylphosphine a commercially available lucirin TPO, that is, 2,4,6-trimethyl- benzoyl-trimethyl phosphine oxide (2,4,6-trimethyl-benzoyl-trimethyl phosphine oxide) can be used.
  • a wider variety of photoinitiators is well specified in Reinh d Schwalm's book "UV Coatings: Basics, Recent Developments and New Application (Elsevier 2007)" p115, and is not limited to the examples described above.
  • the kind of the internal crosslinking agent included in the monomer composition is as described above.
  • the internal crosslinking agent is 0.0005 mol or more
  • black is 0.0005 to 0.002 mol (black is 0.4 parts by weight or more relative to 100 parts by weight of acrylic acid, or 0.4 to 15 parts by weight based on 1 mole of unneutralized acrylic acid contained in the monomer) Can be used in the ratio.
  • black is 0.0005 to 0.002 mol (black is 0.4 parts by weight or more relative to 100 parts by weight of acrylic acid, or 0.4 to 15 parts by weight based on 1 mole of unneutralized acrylic acid contained in the monomer) Can be used in the ratio.
  • black is 0.0005 to 0.002 mol (black is 0.4 parts by weight or more relative to 100 parts by weight of acrylic acid, or 0.4 to 15 parts by weight based on 1 mole of unneutralized acrylic acid contained in the monomer) Can be used in the ratio.
  • black is 0.0005 to 0.002 mol (black is
  • the monomer composition may further include additives such as thickeners, plasticizers, preservative stabilizers, antioxidants, and the like, as necessary.
  • the solvent that can be used at this time can dissolve the above-mentioned components. It can be used without limitation in composition, for example, water, ethane, ethylene glycol, diethylene glycol, triethylene glycol, 1,4-butanediol, propylene glycol, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, Propylene glycol monomethyl ether acetate, methyl ethyl ketone, acetone, methyl amyl ketone, cyclonucleanone, cyclopentanone, diethylene glycol monomethyl ether, diethylene glycol ethyl ether, toluene, xylene, butyrolactone, carbyl It may be used in combination of one or more selected from methyl cellosolve acetate and ⁇ , ⁇ -dimethylacetamide.
  • the solvent may be included in the remaining amount except for the above-described components with respect to the total content of the monomer composition.
  • the hydrogel polymer obtained by thermal polymerization by supplying hot air or by heating the reaction vessel is a semi-ungker, such as a kneader having a stirring shaft, according to the shape of the stirring shaft provided in the reactor.
  • the hydrogel polymer discharged to the outlet may be in the form of several centimeters to several millimeters.
  • the size of the hydrogel polymer obtained may vary depending on the concentration and the injection speed of the monomer composition to be injected, it can be usually obtained a hydrogel polymer having a weight average particle diameter of 2 to 50 mm.
  • the form of the hydrogel polymer generally obtained may be a hydrogel polymer on a sheet having a width of the belt.
  • the thickness of the polymer sheet depends on the concentration and the injection speed of the monomer composition to be injected, but a polymer on the sheet having a thickness of 0.5 to 5 cm can be obtained. It is preferable to feed the monomer composition so that it is.
  • the monomer composition When the monomer composition is supplied to such an extent that the thickness of the polymer on the sheet is too thin, the production efficiency is not preferable, and when the thickness of the polymer on the sheet exceeds 5 cm, the polymerization reaction will not occur evenly over the entire thickness due to the excessively thick thickness. There is a number.
  • the pulverizer used is not limited in configuration, but specifically, a vertical pulverizer, a turbo cutter, a turbo grinder, a rotary cutter mill, a cutting machine Includes any one selected from the group of grinding machines consisting of cutter mills, disc mills, shred crushers, crushers, choppers and disc cutters Although it is possible, it is not limited to the above-mentioned example.
  • the coarse grinding step may be pulverized so that the particle diameter of the hydrogel polymer is 2 to 10mm. ⁇
  • the drying temperature of the drying step may be 150 to 250 ° C. If the drying temperature is less than 150 ° C., the drying time may be too long and the physical properties of the final superabsorbent polymer may be lowered. If the drying temperature is greater than 250 ° C., only the polymer surface is dried excessively. Fine powder may occur in the grinding step, and there is a fear that the physical properties of the superabsorbent polymer to be finally formed decrease. Therefore, preferably, the drying may be performed at a temperature of 150 to 200 ° C, more preferably at a temperature of 170 to 195 ° C.
  • drying time in consideration of the process efficiency, etc., it may proceed for 20 to 90 minutes, but is not limited thereto.
  • the drying method of the drying step is also commonly used as a drying step of the hydrogel polymer, it can be selected and used without limitation of the configuration. Specifically, the drying step may be performed by a method such as hot air supply, infrared irradiation, microwave irradiation, or ultraviolet irradiation.
  • the water content of the polymer after the drying step may be about 0.1 to about 10% by weight.
  • a separate process of classifying the polymer powder obtained after grinding according to the particle diameter may be performed.
  • the polymer having a particle size of 150 to 850 may be classified, and only a polymer powder having such a particle size may be produced through a surface crosslinking reaction step. Since the particle size distribution of the base resin powder obtained through this process has already been described above, further detailed description thereof will be omitted.
  • the horizontal gel strength (G ') before the surface crosslinking of the base resin powder described above It can be stratified in the range of 5,000 Pa or more, or 5,000 to 10,000 Pa, or 5,500 to 8,500 Pa, and if the gel strength of the base resin powder before the surface crosslinking falls within the above range, the superabsorbency prepared through the surface crosslinking reaction described later
  • the resin may achieve the physical properties of one embodiment.
  • the base resin powder may be mixed with hydrophobic inorganic particles in a solid state and treated on a surface thereof, and the treatment method thereof may be a dry treatment and / or a mixing method of a general inorganic powder.
  • the structure also about the method of adding to the surface crosslinking liquid allol base resin powder containing a hydrophilic inorganic particle and a surface crosslinking agent.
  • the surface crosslinking solution and the base resin powder are mixed in a semi-permanent mixture, or the surface crosslinking solution is sprayed onto the base resin powder, and the base resin powder and the surface crosslinking solution are continuously supplied to the mixer which is operated continuously. Method can be used.
  • the hydrophobic inorganic particles and the hydrophilic inorganic particles may be used in amounts of 0.0001 to 0.3 parts by weight, and black of 0.001 to 0.2 parts by weight based on 100 parts by weight of the base resin powder, respectively. Thereby, according to the use of each inorganic particle, the fluid permeability and various characteristics of a super absorbent polymer can be improved more effectively.
  • the superabsorbent polymer of one embodiment prepared using each of the inorganic particles having such a content may also include hydrophobic and hydrophilic inorganic particles in a content range corresponding thereto.
  • the surface crosslinking liquid may further include water and / or a hydrophilic organic solvent as a medium.
  • water and / or a hydrophilic organic solvent as a medium.
  • the surface crosslinking agent and the hydrophilic inorganic particles can be evenly dispersed on the base resin powder.
  • the content of water and hydrophilic organic solvent induces even dispersion of the surface crosslinking agent and the hydrophilic inorganic particles, prevents agglomeration of the base resin powder and at the same time the surface penetration of the surface crosslinking agent
  • the depth can be applied by adjusting the addition ratio to 100 parts by weight of the base resin powder.
  • the surface cross-linking step is the temperature of the reaction to the reaction at the initial temperature of 20 ° C to 130 ° C, black 40 ° C to 120 ° C over 10 minutes to 30 minutes, and the maximum temperature It can be carried out by maintaining the heat treatment for 5 to 60 minutes.
  • the temperature raising means for surface crosslinking reaction is not specifically limited. It can be heated by supplying a heat medium or by directly supplying a heat source.
  • a heated fluid such as steam, hot air, or hot oil may be used, but the present invention is not limited thereto, and the temperature of the heat medium to be supplied may be a means of heating medium, a temperature increase rate, and a target temperature increase.
  • the heat source directly supplied may be a heating method through electricity, a heating method through a gas, but is not limited to the above-described example.
  • the superabsorbent polymer obtained according to the above-described manufacturing method maintains excellent water-absorbing performance such as water-retaining capacity and pressure-absorbing capacity, and satisfies improved horizontal gel strength and liquid permeability, and can satisfy various physical properties of one embodiment.
  • hygiene materials such as diapers, in particular, ultra-thin hygiene materials with reduced pulp content may be appropriately used.
  • a superabsorbent polymer and a method for producing the same, which maintain excellent water absorbing performance such as water-retaining capacity and pressure-absorbing capacity, and which further improves horizontal gel strength and liquid permeability.
  • These super absorbent polymers are diapers.
  • Back sanitary materials in particular, ultra-thin sanitary materials with reduced content of the peel, and the like can be suitably used. [Specific contents to carry out invention]
  • the contact angle with respect to water was measured in the same manner as in the hydrophobic inorganic particles, except that the coating solution dissolved or dispersed in water at a concentration of 20% by weight 0 /. .
  • the particle size was measured according to the European Disposables and Nonwovens Association (EDANA) standard EDANA WSP 220.3 method.
  • EDANA European Disposables and Nonwovens Association
  • the resin of Examples and Comparative Examples W 0 into a (g, about 0.2g) uniformly on the envelope of the non-woven fabric sealed (seal) one after, immersion in physiological saline is a sodium chloride solution of 0.9 weight 0 /.
  • a sodium chloride solution of 0.9 weight 0 /.
  • the envelope was centrifuged and drained at 250 G for 3 minutes, and then the mass W 2 (g) of the envelope was measured.
  • the mass W ⁇ g at that time was measured.
  • W 0 (g) is the initial weight (g) of the superabsorbent polymer
  • W ⁇ g is the weight of the device measured after immersion in physiological saline for 30 minutes without using a super absorbent polymer, and then dehydrated at 250 G for 3 minutes using a centrifuge.
  • W 2 (g) is the weight of the device, including the superabsorbent polymer, after absorbing the superabsorbent polymer in physiological saline at room temperature for 30 minutes and then dehydrating it at 250 G for 3 minutes using a centrifuge.
  • a stainless steel 400 mesh wire was mounted on the bottom of a 60 mm plastic cylinder. Evenly spread the resin W 0 (g, 0.90 g) obtained in Examples 1-6 and Comparative Examples 1-3 on a wire mesh under a temperature of 23 ⁇ 2 ° C. and a relative humidity of 45% and thereon 4.83 kPa (The piston, which can give a uniform load of 0.7 psi), has an outer diameter of slightly smaller than 60 mm, no gap with the inner wall of the cylinder, and unhindered movement of up and down. At this time, the weight W 3 (g) of the apparatus was measured.
  • a glass filter having a diameter of 125 mm and a thickness of 5 mm was placed inside a petri dish having a diameter of 150 mm, and a physiological saline composed of 0.90 weight 0 / .sodium chloride was at the same level as the upper surface of the glass filter.
  • One sheet of filter paper 120 mm in diameter was loaded thereon. The measuring device was placed on the filter paper and the liquid was absorbed for 1 hour under load. After 1 hour, the measuring device was lifted up and the weight W 4 (g) was measured.
  • AUP (g / g) [W 4 (g)-W 3 (g)] / W 0 (g)
  • W 0 (g) is the initial weight (g) of the super absorbent polymer
  • W 3 (g) is the sum of the weight of the superabsorbent polymer and the weight of the device capable of applying a load to the superabsorbent polymer
  • W 4 (g) is the sum of the weight of the superabsorbent resin and the weight of the device capable of applying a load to the superabsorbent resin after absorbing physiological saline to the superabsorbent resin for 1 hour under a load (0.7 psi).
  • the gel strength in the horizontal direction was measured. First, 0.5 g of the superabsorbent polymer samples (30-50 Mesh) of Examples and Comparative Examples were sieved through a sieve. The weighed sample was swollen in 50 g of saline solution for 1 hour. Thereafter, unabsorbed solvent was removed using an aspirator for 4 minutes, and the external solvent was evenly distributed over filter paper and wiped off once.
  • the shear modulus of the linear viscoelastic regime section with a constant storage modulus and a loss modulus while increasing the shear strain Confirmed.
  • 0.1% shear strain is within the linear viscoelastic state section.
  • the storage modulus and loss modulus of the superabsorbent polymer swollen for 60 seconds at the shear strain value of the linear viscoelastic state section were measured, respectively.
  • the storage elasticity obtained at this time was averaged and the horizontal gel strength was calculated
  • the loss modulus is measured to be a very small value compared to the storage modulus.
  • hydrophobic silica particles of VI30S were added to 100 parts by weight of the prepared base resin powder, and the mixture was stirred at room temperature to be mixed so that the base resin powder and the hydrophobic silica particles were mixed well and dried.
  • 0.2 g of an aqueous solution in which hydrophilic silica particles ST-0 were dispersed in water at a concentration of 1 g of ethylene carbonate and 20 weight 0 / ° C was added to 3 g of water, and mixed to prepare a surface crosslinking solution.
  • the surface crosslinking solution was sprayed onto the base resin powder and stirred at room temperature to mix the surface crosslinking solution evenly on the base resin powder.
  • the base resin powder mixed with the surface crosslinking liquid was placed in a surface crosslinking reaction machine, and surface crosslinking reaction was performed.
  • the base resin powder was found to gradually increase in temperature at an initial temperature near 80 ° C., and was manipulated to reach a reaction maximum temperature of 19 C C after 30 minutes. After this reaction peak temperature was reached, the reaction product was further reacted for 15 minutes, and the final prepared superabsorbent polymer sample was taken. After the surface crosslinking process, the superabsorbent polymer of Example 1 having a particle diameter of 150 to 710 / m was prepared by classifying to a standard mesh of ASTM standard.
  • Example 2
  • the superabsorbent polymer of Example 2 was prepared in the same manner as in Example 1 and under the same surface crosslinking conditions, except that 0.05 parts by weight of Aerogel was added instead of the hydrophobic silica particles of I30S. Prepared.
  • Example 3 After the surface crosslinking process, the superabsorbent polymer of Example 2 having a particle size of 150 // m to 710 was prepared by classifying to a standard mesh of ASTM standard.
  • Example 3
  • Example 3 superabsorbent polymer was prepared in the same manner as in Example 1 and under the same surface crosslinking conditions, except that 0.05 part by weight of R972 was added instead of the 130S hydrophobic silica particles. Prepared.
  • Example 4 After the surface crosslinking process, a superabsorbent polymer of Example 3 having a particle size of 150 / im to 710 was prepared by classifying to a standard mesh of ASTM standard.
  • Example 4
  • Base resin powder (gel strength: 6,588 Pa, superabsorbent resin of Example 4 under the same method and same surface crosslinking conditions as Example 1 except that the content of the hydrophobic silica particles of 130S was added at 0.02 parts by weight) was prepared.
  • Example 5 After the surface crosslinking process, the superabsorbent polymer of Example 4 having a particle size of 150 im to 710 was prepared by classifying to a standard mesh of ASTM standard.
  • Example 5
  • Example 6 After the surface crosslinking process, the superabsorbent polymer of Example 5 having a particle diameter of 710 was prepared by classifying to a standard mesh of ASTM standard.
  • Example 6
  • Example of the surface crosslinking with respect to the base resin powder (gel strength: 6,588Pa), the same method as in Example 1 and the same surface crosslinking conditions, except that the amount of the aqueous solution of the hydrophilic silica particles of ST-0 was 0.4g A super absorbent polymer of 6 was prepared.
  • Example 7 After the surface cross-linking process, classified to a standard mesh of ASTM standards 150 The superabsorbent polymer of Example 6 having a particle size of 710 / m was prepared.
  • Example 7
  • Base resin powder (gel strength: except that 0.4g of aqueous solution in which ST-AK hydrophilic silica particles were dispersed in water at a concentration of 20% by weight 0 /.
  • the superabsorbent polymer of Example 7 was prepared in the same manner as in Example 1 and under the same surface crosslinking conditions.
  • Example 7 After the surface crosslinking process, a superabsorbent polymer of Example 7 having a particle size of 150 ⁇ to 710 mm 3 was prepared by classifying to a standard mesh of ASTM standard. Comparative Example 1
  • the superabsorbent polymer of Comparative Example 1 was prepared in the same manner as in Example 1, except that the hydrophobic silica particles and the hydrophilic silica particle aqueous solution were not used during surface crosslinking with respect to the base resin powder (gel strength: 6,588 Pa). .
  • Base resin powder (gel strength: 6,588 Pa, compared with the same method as in Example 1, except that the hydrophobic silica particles were not added and the amount of the hydrophilic silica particles aqueous solution of ST-0 was 0.4 g at the time of surface crosslinking).
  • the super absorbent polymer of Example 2 was prepared.
  • the hydrophobic silica particles of V130S were added in an amount of 0.05 parts by weight, and the surface crosslinking was carried out in the same manner as in Example 1 except that the aqueous hydrophilic silica particles were not used.
  • the superabsorbent polymer of Comparative Example 3 was prepared.
  • the superabsorbent polymer of Comparative Example 6 having a particle size of 150 to 710 was prepared by classifying to a standard mesh of ASTM standard.
  • physical properties of CRC, AUP, SFC, and gel strength (G ′) were measured and evaluated. Physical property values are as shown in Table 2 below.
  • the absorbance value of Equation 1 was calculated and shown in Table 2 together.

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Abstract

La présente invention concerne une résine superabsorbante présentant une perméabilité aux liquides améliorée tout en conservant une excellente performance d'absorption, ainsi que son procédé de production. La résine superabsorbante comporte: une poudre de résine de base comprenant un premier polymère réticulé d'un monomère hydrosoluble à insaturation éthylénique ayant au moins des groupes acides partiellement neutralisés; et une couche superficielle réticulée formée sur la poudre de résine de base et comprenant un second polymère réticulé dans lequel le premier polymère réticulé est réticulé davantage par un carbonate d'alkylène ayant de deux à cinq atomes de carbone. La résine superabsorbante satisfait des propriétés physiques prédéterminées.
PCT/KR2017/000054 2016-03-31 2017-01-03 Résine superabsorbante et son procédé de production WO2017171208A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP17775633.5A EP3336134B1 (fr) 2016-03-31 2017-01-03 Résine superabsorbante et son procédé de production
CN201780003648.6A CN108350188B (zh) 2016-03-31 2017-01-03 超吸收性聚合物及其制备方法
US15/767,903 US10988582B2 (en) 2016-03-31 2017-01-03 Super absorbent polymer and method for preparing same

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KR20160039244 2016-03-31
KR10-2016-0039244 2016-03-31
KR10-2016-0063524 2016-05-24
KR1020160063524A KR101863350B1 (ko) 2016-03-31 2016-05-24 고흡수성 수지 및 이의 제조 방법

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