CN111116816A - Paper diaper with efficient rewet performance and preparation method thereof - Google Patents
Paper diaper with efficient rewet performance and preparation method thereof Download PDFInfo
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- CN111116816A CN111116816A CN201911282620.8A CN201911282620A CN111116816A CN 111116816 A CN111116816 A CN 111116816A CN 201911282620 A CN201911282620 A CN 201911282620A CN 111116816 A CN111116816 A CN 111116816A
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- absorbent resin
- super absorbent
- phosphatidylserine
- rewet
- water
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/15577—Apparatus or processes for manufacturing
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/45—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the shape
- A61F13/49—Absorbent articles specially adapted to be worn around the waist, e.g. diapers
- A61F13/494—Absorbent articles specially adapted to be worn around the waist, e.g. diapers characterised by edge leakage prevention means
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/45—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the shape
- A61F13/49—Absorbent articles specially adapted to be worn around the waist, e.g. diapers
- A61F13/496—Absorbent articles specially adapted to be worn around the waist, e.g. diapers in the form of pants or briefs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/24—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
- A61F2013/530481—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having superabsorbent materials, i.e. highly absorbent polymer gel materials
Abstract
The invention provides a paper diaper with efficient rewet performance and a preparation method thereof, and belongs to the technical field of sanitary products. The invention obtains the super absorbent resin with good salt resistance by grafting the phosphatidylserine to a polyacrylic acid-acrylamide molecular chain, and improves the grafting rate of the phosphatidylserine by optimizing the preparation method. The paper diaper prepared from the super absorbent resin provided by the invention has higher rewet performance.
Description
Technical Field
The invention belongs to the technical field of sanitary articles, and particularly relates to a paper diaper with efficient rewet performance and a preparation method thereof.
Background
In recent years, the market and production of the Chinese paper diaper are greatly developed, but the cost and market permeability of the paper diaper consumed by infants in all years are greatly different from those of developed countries, so that the market development space in China is huge. On one hand, the economy of China continues to grow rapidly, and the development of the baby diapers can be called as a full-aftereffect; on the other hand, the recent policy of two tires in China is coming out, and the development of the diaper market is started first. Therefore, the development space of the paper diaper market in China is extremely considerable. Although the research on the structure of each layer of material of the paper diaper is relatively perfect, the research on the mutual influence among the structures of the layers is less. Through the structural analysis and the performance research of the paper diaper and the analysis of the permeation relation among the structural materials of all layers, a product which can still keep large absorption amount, small reverse osmosis amount, high absorption speed and good diffusion after being used for a long time and under the condition of multiple times of liquid permeation is designed, and the method is the direction of needing further effort at present. The absorption core layer of the paper diaper is a composite core layer which is prepared by physically blending super absorbent resin and fluff pulp according to a certain mass ratio and coating the mixture with wet strength paper or non-woven fabric. The high water absorption resin mainly has the function of absorbing and locking a large amount of water, and the fluff pulp has the function of accelerating the liquid absorption rate and the diffusion speed of liquid in an absorption core layer, and the two functions are mutually complemented. This kind of ingenious layer has strengthened the imbibition speed of panty-shape diapers, has increased the imbibition volume, has increased the volume of keeping liquid, nevertheless also has not enoughly: the diaper is easy to return to seepage after absorbing liquid, and is thick, so that the diaper is easy to break and bunch after absorbing liquid, the water absorption performance is influenced, and the baby feels uncomfortable and the normal life of the baby is influenced.
The prior art, for example, chinese patent No. CN 104684969B, discloses a super absorbent resin which has excellent initial water absorption and does not exude water even when pressure is applied thereto after a certain period of time, and in which the centrifugal separation water retention property (CRC), the pressure water absorption property (AUP), the solution permeability (SFC), the adhesive strength, and the like of the super absorbent resin are all maintained within predetermined ranges to be optimized, thereby improving the physical properties of the final diaper, and thus, a diaper to which the ultra thin technique is applied can be manufactured.
Disclosure of Invention
The invention aims to provide a super absorbent resin and a preparation method thereof, the super absorbent resin is grafted with phosphatidylserine on a polyacrylic acid-acrylamide molecular chain, and can improve the absorption rate and the liquid absorption rate of saline water; the gel strength of the super absorbent resin can be improved, and the pressurized absorption capacity and the liquid retention capacity of saline water are improved; the preparation method can improve the grafting rate of the phosphatidylserine and the liquid absorption performance of the super absorbent resin.
The technical scheme adopted by the invention for realizing the purpose is as follows:
provides a preparation method of super absorbent resin, which comprises the following steps:
s1, mixing cyclohexane, chloro-n-octane, OP100 and Span60, and heating to 50-52 ℃;
s2, taking phosphatidylserine, adding deionized water, carrying out ultrasonic dispersion for 5-8min, and carrying out magnetic stirring for 4-6h to obtain an emulsion;
s3, adding activated carbon into acrylic acid to remove a polymerization inhibitor, adding a NaOH solution into an acrylic acid solution for neutralization after centrifugal separation to prepare an acrylic acid neutralization solution, adding acrylamide, and uniformly mixing;
s4, slowly mixing the solution obtained in the step S3 and the solution obtained in the step S2, adding an initiator and N, N' -methylene bisacrylamide, and uniformly mixing;
s5, slowly dripping the solution obtained in the step S4 into the solution obtained in the step S1 within 15-25min, after dripping is finished, melting nitrogen to react for 33-38min, then heating to 70-72 ℃, reacting for 3-4h, filtering, drying at 70-85 ℃, crushing and sieving. The process of water absorption of superabsorbent resins is a very complicated process. Before water absorption, the polymer network is in a solid network bundle structure, and ion pairs are not ionized. When a macromolecular chain in the polymer network meets water, the hydrophilic group can be hydrated with the water, the hydrophilic group in the polymer network starts to be ionized, the electrostatic repulsion generated between ions in the network can expand the macromolecular network bundle, the concentration difference of the ions inside and outside the network is generated, the osmotic pressure difference inside and outside the network structure is further formed, and water molecules can permeate into the network through osmotic pressure. When the adsorbed water contains salt, the difference in ion concentration is reduced, the osmotic pressure is reduced, and the water absorption capacity is reduced. In a mixed solution of cyclohexane, chloro-n-octane, OP100 and Span60, phosphatidylserine can be grafted on a polyacrylic acid-acrylamide molecular chain, phosphate groups, carboxylic acid groups and amino groups with strong hydrophilicity are introduced, and phosphate ions can be combined with sodium ions and the like in saline water, so that the internal osmotic pressure of the super absorbent resin is increased, the absorption rate and the imbibition rate of the saline water can be improved, and the rewet amount is reduced; two hydrophobic molecular chains are introduced, after the super absorbent resin is contacted with water for water absorption, because the nonpolar hydrophobic chain is not ionized in the water, static charges can not be generated, the hydrophobic chain can not be stretched, and the charged polyacrylic acid molecular chains in the super absorbent resin can be pulled to be closely arranged, so that the gel strength of the super absorbent resin can be improved, the pressurized absorption capacity and the liquid retention capacity of saline water can be improved, and the rewet capacity can be further reduced.
Preferably, the above initiators are sodium peroxodisulfate and guanidine hydrochloride. The redox initiator is composed of an oxidizing agent and a reducing agent, and generates radicals through redox reaction, thereby initiating polymerization reaction. Sodium peroxodisulfate and guanidine hydrochloride are used as initiators, energy generated through redox reaction is large, polyacrylic acid-acrylamide chain free radicals are increased, the grafting rate of phosphatidylserine can be improved, and the higher the grafting rate is, the better the liquid absorption performance of the super absorbent resin is.
Preferably, the phosphatidylserine has a grafting ratio of at least 11.3%.
Provided is a super absorbent resin grafted with phosphatidylserine.
Preferably, the super absorbent resin has a liquid absorption capacity of at least 165(g/g) with respect to saline.
The invention provides application of super absorbent resin in improving the rewet performance of paper diapers.
The invention provides application of phosphatidylserine and chloro-n-octane in preparation of salt-resistant super absorbent resin.
Another object of the present invention is to provide a low rewet diaper comprising: the surface coating layer, the leg opening side leakage prevention separation edges, the flow guide layer, the absorption core layer, the leakage prevention bottom film and the elastic waistline;
the material used for the surface coating layer is selected from one of the following materials: ES hot-air non-woven material, hot-rolled non-woven material, pearl grain three-dimensional composite structure hot-air non-woven material;
the material used by the flow guide layer comprises polylactic acid fiber material;
the leg opening side leakage preventing separation edge is made of SMS non-woven material or PP spun-bonded non-woven material;
the structure of the absorption core is composed of absorbent paper, the super absorbent resin, absorbent paper, fluffy cloth, the super absorbent resin and fluff pulp mixture from top to bottom in sequence;
the material used by the leakproof basement membrane is a PP breathable microporous membrane or a hot-rolled non-woven fabric PE composite basement membrane.
Preferably, the low rewet diaper has a rewet amount of at most 2.8g when the amount of the added saline solution is 200 mL.
The invention has the beneficial effects that:
1) according to the invention, the phosphatidylserine is grafted on the polyacrylic acid-acrylamide, and the phosphate group, the carboxylic acid group and the amino group with strong hydrophilicity are introduced, so that the internal osmotic pressure of the super absorbent resin is increased, the absorption rate and the imbibition rate of saline can be improved, and the rewet amount is reduced; two hydrophobic molecular chains are introduced, after the super absorbent resin is contacted with water for water absorption, because the nonpolar hydrophobic chain is not ionized in the water, static charges can not be generated, the hydrophobic chain can not be stretched, and the charged polyacrylic acid molecular chains in the super absorbent resin can be pulled to be arranged tightly, so that the gel strength of the super absorbent resin can be improved, the pressurized absorption capacity and the liquid retention capacity of saline water can be improved, and the rewet capacity can be further reduced;
2) according to the invention, the initiator is optimized, so that the grafting rate of phosphatidylserine can be improved, the higher the grafting rate is, the higher the salt resistance and gel strength of the super absorbent resin are, and the lower the rewet capacity of the prepared paper diaper is.
Drawings
FIG. 1 is an infrared spectrum of a highly water-absorbent resin in example 1 of the present invention;
FIG. 2 is an infrared spectrum of a polyacrylic acid-acrylamide super absorbent resin in example 1 of the present invention;
FIG. 3 is a graph showing the results of the measurement of the graft ratio in test example 1 of the present invention;
FIG. 4 is a scanning electron micrograph of test example 1 of the present invention;
FIG. 5 is a graph showing the measurement results of the amount of deformation under compression in test example 1 of the present invention;
FIG. 6 shows the results of measurement of liquid-absorbing capacity (Qs), water retention capacity (R), absorbent capacity under pressure (AUL) and liquid-absorbing rate (t) in test example 2 of the present invention;
FIG. 7 shows the results of the measurement of the rewet amount of the diaper in test example 3 of the present invention.
Detailed Description
Unless otherwise indicated, all publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety as if set forth in their entirety.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
When an amount, concentration, or other value or parameter is given as either a range, preferred range, or a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any larger range limit or preferred value and any smaller range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is described, the described range should be construed as including ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. Where numerical ranges are described herein, unless otherwise stated, the stated ranges are intended to include the endpoints of the ranges and all integers and fractions within the ranges.
In addition, the words "a" and "an" preceding an element or component of the invention are intended to mean no limitation on the number of times that the element or component appears (i.e., occurs). Thus, "a" or "an" should be understood to include one or at least one and the singular forms of an element or component also include the plural unless the singular is explicitly stated.
Embodiments of the present invention, including embodiments of the invention described in the summary section and any other embodiments described herein below, can be combined arbitrarily.
The present invention is described in detail below.
Provides a preparation method of super absorbent resin, which comprises the following steps:
s1, mixing 20-25mL of cyclohexane, 0.8-1.2mL of chloro-n-octane, 0.21-0.24mL of OP100 and 0.14-0.15g of span60, and heating to 50-52 ℃;
s2, taking phosphatidylserine, adding deionized water, carrying out ultrasonic dispersion for 5-8min, and carrying out magnetic stirring for 4-6h to obtain an emulsion;
s3, adding activated carbon into acrylic acid to remove a polymerization inhibitor, adding a NaOH solution into an acrylic acid solution for neutralization after centrifugal separation, preparing an acrylic acid neutralization solution with the neutralization degree of 72-76%, adding acrylamide, and uniformly mixing;
s4, slowly mixing the solution obtained in the step S3 and the solution obtained in the step S2, adding an initiator and N, N' -methylene bisacrylamide, and uniformly mixing;
s5, slowly dripping the solution obtained in the step S4 into the solution obtained in the step S1 within 15-25min, after dripping is finished, melting nitrogen to react for 33-38min, then heating to 70-72 ℃, reacting for 3-4h, filtering, drying at 70-85 ℃, crushing and sieving. Preferably, the above acrylic acid: acrylamide: the mass ratio of the phosphatidylserine is 4-5:2-3: 1. Preferably, the N, N' -methylene-bisacrylamide is used in an amount of 0.018 to 0.02% by mass based on the monomer. The process of water absorption of superabsorbent resins is a very complicated process. Before water absorption, the polymer network is in a solid network bundle structure, and ion pairs are not ionized. When a macromolecular chain in the polymer network meets water, the hydrophilic group can be hydrated with the water, the hydrophilic group in the polymer network starts to be ionized, the electrostatic repulsion generated between ions in the network can expand the macromolecular network bundle, the concentration difference of the ions inside and outside the network is generated, the osmotic pressure difference inside and outside the network structure is further formed, and water molecules can permeate into the network through osmotic pressure. When the adsorbed water contains salt, the difference in ion concentration is reduced, the osmotic pressure is reduced, and the water absorption capacity is reduced. In a mixed solution of cyclohexane, chloro-n-octane, OP100 and Span60, phosphatidylserine can be grafted on a polyacrylic acid-acrylamide molecular chain, phosphate groups, carboxylic acid groups and amino groups with strong hydrophilicity are introduced, and phosphate ions can be combined with sodium ions and the like in saline water, so that the internal osmotic pressure of the super absorbent resin is increased, the absorption rate and the imbibition rate of the saline water can be improved, and the rewet amount is reduced; two hydrophobic molecular chains are introduced, after the super absorbent resin is contacted with water for water absorption, because the nonpolar hydrophobic chain is not ionized in the water, static charges can not be generated, the hydrophobic chain can not be stretched, and the charged polyacrylic acid molecular chains in the super absorbent resin can be pulled to be closely arranged, so that the gel strength of the super absorbent resin can be improved, the pressurized absorption capacity and the liquid retention capacity of saline water can be improved, and the rewet capacity can be further reduced.
Preferably, the above initiators are sodium peroxodisulfate and guanidine hydrochloride. Preferably, the above sodium peroxodisulfate: the mass ratio of the guanidine hydrochloride is 1.4-1.8: 1. The redox initiator is composed of an oxidizing agent and a reducing agent, and generates radicals through redox reaction, thereby initiating polymerization reaction. Sodium peroxodisulfate and guanidine hydrochloride are used as initiators, energy generated through redox reaction is large, polyacrylic acid-acrylamide chain free radicals are increased, the grafting rate of phosphatidylserine can be improved, the higher the grafting rate is, the higher the gel strength of the super absorbent resin is, and the higher the absorption rate, the liquid absorption rate, the pressure absorption capacity and the liquid retention capacity of saline water are.
Preferably, the phosphatidylserine has a grafting ratio of at least 11.3%.
Provided is a super absorbent resin grafted with phosphatidylserine.
Preferably, the super absorbent resin has a liquid absorption capacity of at least 165(g/g) with respect to saline.
The invention provides application of super absorbent resin in improving the rewet performance of paper diapers.
The invention provides application of phosphatidylserine and chloro-n-octane in preparation of salt-resistant super absorbent resin.
Another object of the present invention is to provide a low rewet diaper comprising: the surface coating layer, the leg opening side leakage prevention separation edges, the flow guide layer, the absorption core layer, the leakage prevention bottom film and the elastic waistline;
the material used for the surface coating layer is selected from one of the following materials: ES hot-air non-woven material, hot-rolled non-woven material, pearl grain three-dimensional composite structure hot-air non-woven material;
the material used by the flow guide layer comprises polylactic acid fiber material;
the leg opening side leakage preventing separation edge is made of SMS non-woven material or PP spun-bonded non-woven material;
the structure of the absorption core is composed of absorbent paper, the super absorbent resin, absorbent paper, fluffy cloth, the super absorbent resin and fluff pulp mixture from top to bottom in sequence;
the material used by the leakproof basement membrane is a PP breathable microporous membrane or a hot-rolled non-woven fabric PE composite basement membrane.
Preferably, the surface coating layer is made of ES hot air non-woven material, the leg opening side leakage prevention separation edge is made of SMS non-woven material, and the leakage prevention bottom film is made of PP breathable microporous film.
Preferably, the low rewet diaper has a rewet amount of at most 2.8g when the amount of the added saline solution is 200 mL.
The present invention is further described in detail with reference to the following examples:
example 1:
a preparation method of super absorbent resin comprises the following steps:
1) 20mL of cyclohexane, 1mL of chloro-n-octane, 0.22mL of OP100 and 0.14g of Span60 were mixed and heated to 50 ℃;
2) taking 2g of phosphatidylserine, adding 30mL of deionized water, carrying out ultrasonic dispersion for 5-8min, and carrying out magnetic stirring for 4-6h to obtain an emulsion;
3) adding activated carbon into acrylic acid to remove a polymerization inhibitor, performing centrifugal separation, then dropwise adding 10 wt% NaOH solution into 20g of 50 wt% acrylic acid solution for neutralization, controlling the dropwise adding speed to be 1 drop/s, preparing acrylic acid neutralizing solution with the neutralization degree of 75%, adding 6g of acrylamide for dissolution, and uniformly mixing;
4) slowly mixing the solution obtained in the step 3) and the solution obtained in the step 2), adding 0.72g N, N' -methylene bisacrylamide (NMBA) solution (0.5 wt%), stirring uniformly, adding 0.028g of sodium persulfate and 0.019g of guanidine hydrochloride, and stirring uniformly;
5) slowly dripping the solution obtained in the step S4 into the solution obtained in the step S1 within 20min, melting nitrogen to react for 35min after dripping is finished, heating to 70 ℃, reacting for 3.5h, filtering, drying at 85 ℃, crushing, and sieving with a 100-mesh sieve.
Mixing the prepared mixture with the mixture in a ratio of 1:60, fully grinding the mixture in an agate mortar, putting a proper amount of ground sample into a tabletting mold to be pressed into tablets, and analyzing the tablets in a Fourier transform infrared spectrometer (FTIR). The infrared spectrum of the super absorbent resin is shown in figure 1. FIG. 2 is an infrared spectrum of polyacrylic acid-acrylamide super absorbent resin.
As can be seen from the comparison of FIGS. 1 and 2, 3427cm is present in both FIGS. 1 and 2-12949cm at the peak of O-H, N-H stretching vibration-1Is at the C-H stretching vibration peak of 1664cm-1para-CONH2Middle C ═ O stretching vibration peak, 1560cm-1para-CONH2Middle N-H bending vibration peak, 1448cm-1C ═ O stretching vibration peak at-COO-, 1403cm-1、1320cm-1The part is a double absorption peak generated by coupling of stretching vibration of C-O in-COO-and bending vibration of O-H, N-H, so that the polyacrylic acid-acrylamide super absorbent resin is successfully synthesized through experiments. 3427cm in FIG. 1-12949cm at the peak of N-H stretching vibration-11448cm at C-H telescopic vibration peak-1C ═ O stretching vibration peak at-COO-, 1403cm-1The stretching vibration peak of C-O in-COO-is enhanced, and 1735cm is also existed-1Stretching vibration peak of 1204cm at C ═ O-1Stretching vibration peak of ester group C-O-C, 1222cm-1To PO2 -Antisymmetric telescopic vibration peak, 1086cm-1To PO2 -Symmetric telescopic vibration peak, 1062cm-1The P-O-C stretching vibration peak is shown, which indicates that the phosphatidyl silk is successfully grafted on the polyacrylic acid-acrylamide(ii) an amino acid.
Example 2:
a low rewet diaper comprising: surface coating layer, leg mouth side leakage preventing separation edge, flow guide layer, absorption core layer, leakage preventing basement membrane, and elastic waistline.
Selecting ES hot-air non-woven fabric to make a surface coating layer; selecting a polylactic acid fiber material to manufacture a flow guide layer; selecting SMS non-woven materials to manufacture the materials for the leg opening side leakage prevention separation edges; the structure of the absorption core is composed of absorbent paper, the super absorbent resin prepared by the invention, absorbent paper, fluffy cloth, the super absorbent resin prepared by the invention and fluff pulp mixture from top to bottom in sequence; the PP breathable microporous film is selected to manufacture the leakage-proof basement membrane.
The preparation method of the paper diaper comprises the following steps:
preparation of an absorption core layer: according to the interlayer design proportion, a layer of hot melt adhesive is applied to the surface of the absorbent paper (glue application temperature: 140 ℃), then SAP is uniformly sprayed and adhered to the absorbent paper, and the absorbent paper/SAP/absorbent paper composite material is prepared after the SAP is placed in a calender and is subjected to calendering molding (roll temperature: 120 ℃). Demoulding and molding the hot air fluffy cloth, coating the hot air fluffy cloth with an SAP fluff pulp mixture (mass ratio is 1:1) and a water-absorbent paper/SAP/water-absorbent paper composite material (the temperature of hot melt adhesive applied to a coating layer is 140 ℃), compacting and cutting to prepare the absorption core layer.
Preparing the paper diaper: gluing and compounding the surface coating layer and the flow guide layer (gluing temperature: 140 ℃), applying leg opening side leakage prevention separation edges and left and right stickers on the surface layer to manufacture a compound surface layer, and simultaneously compounding the leakage prevention bottom film, the polyethylene breathable cast film, the front waist sticker and the elastic waistline on line to manufacture a compound bottom film; and compounding the composite surface layer, the absorption core layer and the composite bottom film on line, compacting and cutting into a finished diaper.
Comparative example 1:
the preparation process of the super absorbent resin is not added with chloro-n-octane, and the rest is completely the same as that of the example 1.
Comparative example 2:
the preparation process of the super absorbent resin does not add phosphatidylserine, and the rest is completely the same as that of the example 1.
Comparative example 3:
the preparation process of the super absorbent resin does not add chloro-n-octane and phosphatidylserine, and the rest is completely the same as that of the example 1.
Comparative example 4:
the initiators used in the preparation of the superabsorbent resin were sodium peroxodisulfate and sodium bisulfite, the remainder being identical to that of example 1.
Comparative example 5:
the initiators used in the preparation of the super absorbent resin were potassium persulfate and guanidine hydrochloride, and the rest was identical to that of example 1.
Comparative example 6:
the initiators used in the preparation of the super absorbent resin were potassium persulfate and sodium bisulfite, and the rest was identical to that of example 1.
Test example 1:
1.1 determination of the graft ratio: and (3) measuring the grafting rate of the phosphatidylserine by adopting an infrared spectrum method. The results of the graft ratio measurement are shown in FIG. 3.
As can be seen from fig. 3, the grafting ratio of comparative examples 1, 2, 3 was almost 0 and phosphatidylserine was not grafted to the super absorbent resin, compared to examples 1, 4, 5, 6, which indicates that phosphatidylserine can be grafted to polyacrylic acid-acrylamide in the cyclohexane, chloro-n-octane, OP100, Span60 mixed solution containing chloro-n-octane; the grafting ratio in example 1 is significantly higher than that in comparative examples 4, 5 and 6, which shows that the energy generated by redox reaction is larger by using sodium peroxodisulfate and guanidine hydrochloride as initiators, so that the free radical of polyacrylic acid-acrylamide chain is increased, and the grafting ratio of phosphatidylserine can be improved.
1.2 scanning electron microscopy analysis: the appearance of the outer layer of the super absorbent resin is measured by a galvanometer scanner (JSM-5600LV), and the acceleration voltage is 20 kV. The resin was fully swollen in distilled water before testing, frozen in liquid nitrogen and then vacuum dried on a freeze dryer for 48 h. The scanning electron micrograph is shown in FIG. 4.
As can be seen from FIG. 4, compared with comparative example 6 and example 1, the resin of comparative example 3 continuously absorbs water after contacting with water, the resin continuously expands, and the weak part on the surface is broken and torn, and compared with comparative example 6, the internal grid of the water-absorbent resin of example 1 is tighter, which shows that after contacting with water and absorbing water, the introduced nonpolar hydrophobic chain can pull the charged polyacrylic acid molecular chain in the super-absorbent resin, so that the molecular chain is tightly arranged, and the higher the grafting rate of phosphatidylserine is, the tighter the charged polyacrylic acid molecular chain in the super-absorbent resin after absorbing water is.
1.3 determination of gel Strength: taking 2g of resin, and completely swelling the resin to obtain saturated gel; spreading the gel in a glass dish, placing the glass slide on the gel, measuring the height of the upper edge of the glass slide by using a height measuring instrument, and recording the reading L0(ii) a The 50g weight was then placed on the slide while timing, and the height L of the upper edge of the slide was recorded every 30s, repeated three times, and the average was taken. The deformation resistance of the resin hydrogel,. DELTA.L ═ L (L) was obtained0-L). The gel strength of the resin is relatively characterized by the amount of deformation under compression. The measurement results of the deformation resistance amount are shown in FIG. 5.
As can be seen from FIG. 5, the deformation resistance of the super absorbent resin of example 1, comparative example 4, comparative example 5 and comparative example 6 is obviously smaller than that of the super absorbent resin of comparative example 1, comparative example 2 and comparative example 3, and the deformation resistance of the super absorbent resin of example 1 is obviously smaller than that of the super absorbent resin of comparative example 4, comparative example 5 and comparative example 6, which shows that after the super absorbent resin grafted with phosphatidylserine is contacted with water for water absorption, the introduced nonpolar hydrophobic chain can pull charged polyacrylic acid molecular chains in the super absorbent resin, so that the molecular chains are arranged tightly, the gel strength of the super absorbent resin is improved, and the higher the grafting ratio of the phosphatidylserine is, the higher the gel strength of the super absorbent resin is.
Test example 2:
2.1 determination of the imbibition Rate: placing SAP with mass m (about 0.2 g) at the bottom of tea bag, dispersing uniformly, sealing tea bag, soaking in sufficient 0.9% sodium chloride solution, absorbing the solution for 30min, taking out tea bag, standing, draining for 10min, and weighing its weight m1(ii) a Blank comparisons were made with tea bags without samples,weighing blank experiment tea bags with mass m2. The amount of SAP absorbed Qs was calculated according to the following formula:
Qs(g/g)＝(m1-m2)/m
wherein m is the mass of the SAP sample, m1Mass m after absorption of the solution for the tea bag containing SAP2Is the quality of the tea bag after water absorption in the blank experiment.
2.2 determination of Water Retention: mass m is takenRPlacing (about 0.2 g) SAP at the bottom of tea bag, dispersing uniformly, sealing the tea bag, soaking in sufficient 0.9% sodium chloride solution, maintaining the immersed state for 30min, taking out the tea bag, centrifuging (centrifugal force 250g) in centrifuge for 3min, and weighing mR1(ii) a Performing blank comparison with tea bags without samples, centrifuging, and weighing blank tea bags with mass mR2. The water retention R of the SAP was calculated according to the following formula:
R(g/g)＝(mR1-mR2)/mR
in the formula, mRMass of SAP sample, mR1Mass m after centrifugation of the tea bag containing SAPR2Is the quality of the blank experiment tea bag after centrifugation.
2.3 measurement of the amount of absorption under pressure: the measuring method and the device refer to the national standard GB/T2222905-. Weighing mA(about 0.4 g) of a super absorbent resin was uniformly scattered on the bottom of the cylinder, a spacer and a weight of 200g were put in the cylinder, and the mass m was weighedA1. Placing the cylinder into a culture dish containing a proper amount of 0.9% sodium chloride solution, standing for 60min, and weighing the cylinder againA2. The absorbency under pressure AUL of SAP is calculated according to the following formula:
AUL(g/g)＝(mA2-mA1)/mA
in the formula, mAIs the mass of the SAP sample; m isA1To measure the mass of the device for measuring the amount of pressure absorbed; m isA2The mass of the device for measuring the pressure absorption capacity after the solution is sucked.
2.4 determination of the imbibition Rate: adding 25mm iron core tetrafluoro stirrer and 50g sodium chloride solution with the mass fraction of 0.9% into a 100mL beaker, placing the beaker on a magnetic stirrer, keeping the temperature constant at about 25 ℃, starting stirring, controlling the rotating speed at 1500r/min, then pouring 2g SAP into the beaker, starting timing by a timer, and taking the time t for the vortex of the solution in the beaker to disappear as the liquid absorption rate of a sample.
The measurement results of the liquid-absorbing capacity (Qs), water retention capacity (R), pressurized absorption capacity (AUL), and liquid-absorbing rate (t) are shown in FIG. 6.
As can be seen from fig. 6, Qs, R, AUL of example 1, comparative example 4, comparative example 5, comparative example 6 are significantly higher than those of comparative example 1, comparative example 2, comparative example 3, t is significantly lower than those of comparative example 1, comparative example 2, comparative example 3, which shows that the super absorbent resin grafted with phosphatidylserine introduces hydrophilic phosphate group, carboxylic acid group, amino group, so that the ion density inside the network of the super absorbent resin is increased, and sodium ion and the like in the salt solution are combined with phosphate ion, so that the internal osmotic pressure of the super absorbent resin is increased, and the absorption rate of the super absorbent resin to saline can be increased, and the liquid absorption rate is increased; the introduction of the nonpolar hydrophobic chain can improve the gel strength of the super absorbent resin and increase the pressurized absorption capacity and the liquid retention capacity of saline. Qs, R and AUL in example 1 are obviously higher than those in comparative examples 4, 5 and 6, and t is obviously lower than those in comparative examples 4, 5 and 6, which shows that the higher the grafting ratio of phosphatidylserine, the higher the absorption capacity to saline, the higher the absorption rate under pressure, and the higher the liquid retention amount.
Test example 3:
testing the rewet amount of the paper diaper: cutting off the protective rubber band of the diaper sample, placing the diaper sample on a liquid permeation comprehensive tester, measuring 200mL of physiological saline, quickly pouring the physiological saline into a funnel, placing enough filter paper on the surface of the diaper after 5min of liquid discharge, pressing a standard pressing block with the diameter of 100mm and the mass of (1.2 +/-0.02) kg, timing, and reading the result to be accurate to 0.01g after 1 min. The test results of the rewet amount of the diaper are shown in FIG. 7.
As can be seen from fig. 7, the rewet amount of the diapers prepared from the super absorbent resins prepared in example 1, comparative example 4, comparative example 5 and comparative example 6 is significantly lower than that of comparative example 1, comparative example 2 and comparative example 3, and example 1 is significantly lower than that of comparative example 4, comparative example 5 and comparative example 6, which shows that the grafted phosphatidylserine can increase the absorption rate, liquid absorption rate, pressure absorption amount and liquid retention amount of the super absorbent resin to saline, thereby reducing the rewet amount of the diapers prepared, and the higher the grafting ratio of phosphatidylserine, the less the rewet amount of the diapers prepared.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (9)
1. A preparation method of super absorbent resin is characterized by comprising the following steps:
s1, mixing cyclohexane, chloro-n-octane, OP100 and Span60, and heating to 50-52 ℃;
s2, taking phosphatidylserine, adding deionized water, carrying out ultrasonic dispersion for 5-8min, and carrying out magnetic stirring for 4-6h to obtain an emulsion;
s3, adding activated carbon into acrylic acid to remove a polymerization inhibitor, adding a NaOH solution into an acrylic acid solution for neutralization after centrifugal separation to prepare an acrylic acid neutralization solution, adding acrylamide, and uniformly mixing;
s4, slowly mixing the solution obtained in the step S3 and the solution obtained in the step S2, adding an initiator and N, N' -methylene bisacrylamide, and uniformly mixing;
s5, slowly dripping the solution obtained in the step S4 into the solution obtained in the step S1 within 15-25min, after dripping is finished, melting nitrogen to react for 33-38min, then heating to 70-72 ℃, reacting for 3-4h, filtering, drying at 70-85 ℃, crushing and sieving.
2. The method of claim 1, wherein: the initiator is sodium peroxodisulfate and guanidine hydrochloride.
3. The method of claim 2, wherein: the grafting ratio of the phosphatidylserine is at least 11.3%.
4. Use of phosphatidylserine and chloro-n-octane in the preparation of salt-resistant super absorbent resin.
5. A super absorbent resin grafted with phosphatidylserine is characterized in that: prepared by the process of claim 1 or 2.
6. The super absorbent resin according to claim 5, wherein: the super absorbent resin has a liquid absorption capacity of at least 165(g/g) for saline.
7. Use of the super absorbent resin according to claim 5 or 6 for improving rewet performance of diapers.
8. A low rewet diaper comprising: the surface coating layer, the leg opening side leakage prevention separation edges, the flow guide layer, the absorption core layer, the leakage prevention bottom film and the elastic waistline;
the material used for the surface coating layer is selected from one of the following materials: ES hot-air non-woven material, hot-rolled non-woven material, pearl grain three-dimensional composite structure hot-air non-woven material;
the material used by the flow guide layer comprises a polylactic acid fiber material;
the leg opening side leakage preventing separation edges are made of SMS non-woven materials or PP spun-bonded non-woven materials;
the structure of the absorbent core is sequentially from top to bottom of absorbent paper, the super absorbent resin as claimed in claim 5, absorbent paper, fluffy cloth, the super absorbent resin as claimed in claim 5 and fluff pulp mixture;
the material used by the leakproof basement membrane is a PP breathable microporous membrane or a hot-rolled non-woven fabric PE composite basement membrane. .
9. A low rewet diaper as claimed in claim 8, wherein: the rewet amount of the low-rewet diaper is at most 2.8g when the saline adding amount is 200 mL.
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