CN116421766B - Preparation method of liquid sanitary towel absorption core - Google Patents

Preparation method of liquid sanitary towel absorption core Download PDF

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Publication number
CN116421766B
CN116421766B CN202310408413.2A CN202310408413A CN116421766B CN 116421766 B CN116421766 B CN 116421766B CN 202310408413 A CN202310408413 A CN 202310408413A CN 116421766 B CN116421766 B CN 116421766B
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water phase
alkyl
acrylic
surfactant
acrylate
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CN116421766A (en
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范鉴全
熊育资
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Procter and Gamble Co
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Guangzhou Anjie Core Material Technology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS 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
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F13/15Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/15577Apparatus or processes for manufacturing
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS 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
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F13/15Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/53Absorbent 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
    • A61F13/534Absorbent 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 an inhomogeneous composition through the thickness of the pad
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/20Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/24Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/425Porous materials, e.g. foams or sponges
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/48Surfactants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS 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
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F13/15Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F2013/16Sanitary towels; Means for supporting or fastening them
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention provides a preparation method of a liquid sanitary towel absorption core body, which comprises the following steps: s1, mixing an acrylic ester monomer 1, a cross-linking agent, a photoinitiator and a surfactant to obtain an oil phase 1, and then adding a water phase A and a water phase B to obtain HIPE emulsion 1; s2, mixing an acrylic ester monomer 2, a cross-linking agent, a photoinitiator and a surfactant to obtain an oil phase 2, and then adding a water phase C and a water phase D to obtain HIPE emulsion 2; s3, coating HIPE emulsion 1 and HIPE emulsion 2 on cloth, and carrying out dehydration, drying and slitting after illumination and steam treatment to obtain a liquid sanitary towel absorption core; wherein the surfactant is obtained by reacting amino alkyl acrylate with haloalkane and/or haloalkane derivative. The invention improves the liquid transmission capacity, ensures that the product has the effects of high-efficiency absorption and lasting dryness, overcomes the defects existing in the prior art, and has good application prospect.

Description

Preparation method of liquid sanitary towel absorption core
Technical Field
The invention belongs to the technical field of foam material absorption cores, and particularly relates to a preparation method of a liquid sanitary towel absorption core.
Background
The liquid sanitary towel is called as the liquid sanitary towel because the raw material of the absorbent core body is derived from the liquid material, and the product has the characteristics of light weight, air permeability, zero touch, dryness, quick absorption and the like compared with the traditional sanitary towel. Although the name of the sanitary towel is liquid, the sanitary towel does not contain liquid or cotton, but adopts a microporous absorbent material made of novel technology, and the absorbent core is characterized by being full of holes (high porosity), being light and thin and being convenient for ventilation, and being capable of automatically absorbing fluid, so that the risk of SAP particles in the traditional sanitary towel product is avoided.
However, most of the existing liquid sanitary towel products have side leakage, easy rewet and other problems, the absorption effect has a large defect, the absorbed liquid cannot be efficiently transferred, the effects of quick absorption and lasting dryness are difficult to realize, and the use requirements of markets and users cannot be met.
In view of the foregoing, there is a need to develop a new technical solution to solve the problems existing in the prior art and meet the development requirements of the current market.
Disclosure of Invention
The term "HIPE emulsion" as used herein refers to high internal phase emulsions.
Based on the method, the acrylate monomer, the cross-linking agent, the initiator and the specific surfactant are mixed to obtain the absorption core with stronger absorption performance after reaction, and meanwhile, the upper layer and the lower layer of the absorption core have different pore sizes, so that the product can generate good capillary action, the liquid transfer capacity is further improved, the product has the effects of high-efficiency absorption and lasting dryness, the defects in the prior art are overcome, and the method has good application prospect.
An object of the present invention is to provide a method for preparing an absorbent core for a liquid sanitary napkin, comprising the steps of:
s1, mixing an acrylic ester monomer 1, a cross-linking agent, a photoinitiator and a surfactant to obtain an oil phase 1, and then adding a water phase A comprising inorganic salt and a water phase B comprising the initiator and acrylic acid salt and/or acrylic sulfonate and derivatives thereof to obtain HIPE emulsion 1;
s2, mixing an acrylic ester monomer 2, a cross-linking agent, a photoinitiator and a surfactant to obtain an oil phase 2, and then adding a water phase C comprising inorganic salt and a water phase D comprising the initiator, acrylic acid salt and/or acrylic sulfonate and derivatives thereof to obtain HIPE emulsion 2;
s3, respectively coating the HIPE emulsion 1 and the HIPE emulsion 2 on the upper surface and the lower surface of cloth, and dehydrating and drying after the treatments of illumination and steam to obtain the liquid sanitary towel absorption core;
wherein,,
the surfactant is obtained by reacting acrylic amino alkyl ester and/or acrylic amino alkyl ester derivative with haloalkane and/or haloalkane derivative;
the inorganic salt is selected from one or more of alkaline earth metal chloride or sulfate and alkali metal chloride or sulfate;
the cloth is selected from one of woven cloth or non-woven cloth.
Specifically, the acrylic aminoalkyl esters of the present invention generally refer to acrylic aminoalkyl esters having two alkyl segments attached, including, but not limited to, dimethylaminoalkyl (meth) acrylate, diethylaminoalkyl (meth) acrylate, dipropylaminoalkyl (meth) acrylate, dibutylaminoalkyl (meth) acrylate, and the like.
Further, in the acrylic amino alkyl ester and/or acrylic amino alkyl ester derivative, the alkyl in the alkyl ester is selected from C1-C20 alkyl; the amino group is-N (R) 1 )(R 2 ) The R is 1 And R is 2 Independently selected from a hydrogen atom or a C1-C20 alkyl group;
in the amino alkyl acrylate derivative,
one or more hydrogen atoms on the acrylic group are substituted with one or more of a fluorine atom, a chlorine atom, a bromine atom, an iodine atom, or a C1-C20 alkyl group;
and/or the number of the groups of groups,
one or more carbon atoms in the alkyl group are replaced by one or more of polyethylene glycol, polypropylene glycol and polytetramethylene glycol chain segments;
and/or the number of the groups of groups,
the c=c double bond on the acrylic group can be reduced, oxidized or added to a different group.
Further, the preparation method of the surfactant comprises the following steps:
adding acrylic amino alkyl ester and/or acrylic amino alkyl ester derivative, alkyl halide and/or alkyl halide derivative and polymerization inhibitor into solvent, heating and stirring at 40-60 ℃ for reacting for 20-30h, and purifying to obtain the surfactant.
The surfactant prepared by the invention can form micelle in solution, greatly reduces surface tension, has good emulsifying capacity, and promotes each component in emulsion to be dispersed in a system more uniformly and stably. Surprisingly, it was found that the surfactant does not affect the crosslinked structure as an impurity in the polymerization reaction, and has a better effect than the conventional surfactant, and since the component contains an acrylic acid structure, it can participate in the polymerization reaction, and by adjusting the content of each component, it can achieve the technical effect of adjusting the pore size of the absorbent core after reacting with acrylic acid salt, acrylic acid monomer having a long chain structure, and the crosslinking agent. The upper layer in the absorption core body is large holes, the lower layer is small holes, and capillary action is realized, so that liquid can be quickly permeated into the lower layer, blood can be quickly and evenly dispersed and stored in the bottom layer, the situation that the blood is not accumulated on the surface layer of the sanitary towel can be ensured, and the problem of side leakage can be effectively solved.
Further, in the haloalkane and/or haloalkane derivative, a halogen atom is selected from one of a fluorine atom, a chlorine atom, a bromine atom and an iodine atom; the carbon number of the alkyl group is selected from 14 to 25;
in the halogenated alkyl derivative, one or more carbon atoms on the alkyl are substituted by one or more of hydrogen atoms, oxygen atoms, alkenyl groups, alkynyl groups, aryl groups, hydroxyl groups, amino groups, carbonyl groups, carboxyl groups, ester groups, cyano groups and nitro groups;
and/or the number of the groups of groups,
in the haloalkane derivative, one or more hydrogen atoms on an alkyl group are replaced by one or more of fluorine atoms, chlorine atoms, bromine atoms and iodine atoms;
and/or the number of the groups of groups,
in the halogenated alkyl derivative, a halogen atom is substituted by one or more of a sulfonate group and a methylsulfonic acid group.
Further, the method comprises the steps of,
in the step S1, the mass ratio of the acrylic ester monomer 1 to the cross-linking agent to the photoinitiator to the surfactant is (40-100): 5-40): 0.05-2): 2-10; in the water phase A, the mass fraction of inorganic salt is 1-4%; in the water phase B, the mass fraction of the initiator is 0.1-10%, and the mass fraction of the acrylate and/or the acrylate sulfonate and the derivative thereof is 0.1-5%; the volume ratio of the oil phase 1 to the water phase A to the water phase B is 1 (20-40): 1-10;
in the step S2, the mass ratio of the acrylic ester monomer 2 to the cross-linking agent to the photoinitiator to the surfactant is (40-100): 5-40): 0.05-2): 2-10; in the water phase C, the mass fraction of the inorganic salt is 1-4%; in the water phase D, the mass fraction of the initiator is 0.1-10%, and the mass fraction of the acrylate and/or the acrylate sulfonate and the derivative thereof is 0.1-5%; the volume ratio of the oil phase 2 to the water phase C to the water phase D is 1 (28-40): 1-10.
Further, the HIPE emulsion 1 and HIPE emulsion 2 were prepared using a continuous emulsification apparatus.
Further, the acrylic acid ester monomer 1 and the acrylic acid ester monomer 2 are acrylic acid alkyl ester or methacrylic acid alkyl ester, and the alkyl in the acrylic acid alkyl ester or the methacrylic acid alkyl ester is selected from C4-C20 alkyl.
Further, the cross-linking agent is selected from one or more of ethylene glycol diacrylate, ethylene glycol dimethacrylate, butylene glycol diacrylate, hexylene glycol dimethacrylate, trimethylol triacrylate, tripropylene glycol diacrylate, trimethylol trimethacrylate and tripropylene glycol dimethacrylate.
Further, in step S3, the light has a wavelength of 205-450nm and an intensity of 40-1000mW/cm 2 The time is 5-180s.
Further, the initiator is selected from one or more of ammonium persulfate, sodium persulfate, potassium persulfate and azo initiator.
Further, the photoinitiator is preferably one or more of benzophenone, benzil, thioxanthone, benzyl ketal, α -hydroxyalkyl benzophenone, α -aminoalkylbenzophenone, and acylphosphine oxide.
Further, the acrylic acid salt and/or the acrylic sulfonate comprises sodium acrylate, sodium methacrylate sulfonate and sodium acrylate sulfonate, and the mass parts of the sodium acrylate, the sodium methacrylate sulfonate and the sodium acrylate sulfonate are 0.1-50 parts.
The invention has the beneficial effects that:
1. according to the invention, a specific surfactant is compounded with a long-chain acrylic ester monomer and a cross-linking agent, and an absorption core body with stronger adsorption performance is prepared according to a HIPE synthesis process and method, so that the product has higher porosity and a compact micropore structure, a 3D three-dimensional fluid storage function is realized, the surface of the sanitary towel can be kept dry and comfortable, the service time of the sanitary towel is prolonged, and the problems of pressure blood rewet and side leakage of the traditional core body material are solved.
2. According to the invention, the hole sizes of the materials of each layer of the core body are optimally designed according to the fluid characteristics of human blood, so that the upper layer of the absorption core body is a large-aperture absorption layer with the diameter of 30-60 mu m, the absorption core body is suitable for quickly absorbing fluid, and the liquid can be quickly permeated to the lower layer; the lower layer is a small-aperture absorbing foam layer with the diameter of 1-15 mu m, is suitable for dispersing and storing aqueous fluid, can rapidly and evenly disperse the fluid on the bottom layer, and meanwhile, according to the capillary action principle, the size of the hole of the lower layer is obviously smaller than that of the hole of the upper layer, so that the small hole of the lower layer of the core body can more efficiently transfer and absorb the upper layer fluid, and the upper layer can be kept dry.
Drawings
Fig. 1 is an SEM image of the upper and lower layers of the absorbent core of the liquid sanitary napkin prepared in example 1 of the present invention.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are set forth. The starting materials, reactions and workup procedures used in the examples are those commonly practiced in the market and known to those skilled in the art unless otherwise indicated.
The initiator in the embodiment of the invention is ammonium persulfate.
The photoinitiator in the present example was 1-hydroxycyclohexyl phenyl ketone (photoinitiator 184).
In the embodiment of the invention, "parts" refer to parts by weight.
Example 1
A method for preparing an absorbent core of a liquid sanitary napkin, comprising the steps of:
s0. adding dimethylaminoethyl methacrylate, 1-chlorodocosane (dimethylaminoethyl methacrylate: 1-chlorodocosane=1:1, n/n) and trace polymerization inhibitor (phenothiazine) into acetone, stirring at 50deg.C for reacting for 20h, centrifuging, washing, and drying to obtain surfactant;
s1, mixing 55 parts of eicosanoate, 20 parts of ethylene glycol dimethacrylate, 1 part of a photoinitiator and 5 parts of the surfactant to obtain an oil phase 1, and then adding a water phase A containing 2% of calcium chloride by mass and a water phase B containing 7% of an initiator by mass, 0.5% of sodium acrylate, 0.5% of sodium methacrylate sulfonate and 0.5% of sodium acrylate, wherein the volume ratio of the oil phase 1 to the water phase A to the water phase B is 1:26:1 to obtain HIPE emulsion 1;
specifically, in the continuous emulsifying device, an oil phase is prepared in an oil phase material storage tank, an inorganic salt water phase is prepared in an aqueous phase material storage tank, an initiator aqueous phase is prepared in an initiator storage tank, when the emulsifying device stably operates, the emulsion part of primary mixing emulsification in a first static mixer module is controlled by a first backflow constant flow pump to be conveyed back to a first emulsifying kettle, and the emulsion part of secondary mixing emulsification in a second static mixer module is controlled by a second backflow constant flow pump to be conveyed back to a second emulsifying kettle; the flow of the reflux is precisely controlled by a first reflux constant flow pump, and meanwhile, the oil phase in an oil phase material storage tank and the water phase in a water phase material storage tank are respectively and continuously conveyed into a first emulsifying kettle through an oil phase feeding constant flow pump and a water phase feeding constant flow pump to be premixed with the emulsion in the kettle which is being mixed and emulsified to obtain a premixed material, and the premixed material is conveyed into a first static mixer module to be mixed and emulsified to obtain a premixed emulsion I with the water-oil ratio of 14:1;
the first premixed emulsion is respectively partially conveyed into a first emulsifying kettle through a first backflow constant flow pump and is conveyed into a second emulsifying kettle through a first premixed emulsion feeding constant flow pump and a control, the first premixed emulsion in the first premixed emulsion feeding constant flow pump and the water phase continuously conveyed into the second emulsifying kettle through the water phase feeding constant flow pump are premixed and combined to obtain a premixed material, and the premixed material is conveyed into a second static mixer module to be mixed and emulsified to obtain a second premixed emulsion; the premixed emulsion II is respectively and partially conveyed into a second emulsifying kettle through a second reflux constant flow pump control, is conveyed to a third static mixer module through a constant flow pump and control, and is finally mixed and emulsified with an initiator water phase which is continuously conveyed through an initiator feeding constant flow pump control, and HIPE emulsion 1 is obtained after mixed and emulsified, and is continuously conveyed to the next procedure through an emulsified product output interface;
s2, mixing 40 parts of isooctyl acrylate, 10 parts of ethylene glycol dimethacrylate, 1 part of a photoinitiator and 2 parts of the surfactant to obtain an oil phase 2, and then adding a water phase C containing 1% of calcium chloride by mass and a water phase D containing 8% of an initiator by mass, 0.5% of sodium acrylate, 0.5% of sodium methacrylate sulfonate and 0.5% of sodium acrylate sulfonate, wherein the volume ratio of the oil phase 2 to the water phase C to the water phase D is 1:31:1 to obtain HIPE emulsion 2;
the HIPE emulsion 2 was treated in a continuous emulsification apparatus as described in S1;
s3, coating the HIPE emulsion 1 on the lower surface of a non-woven fabric, wherein the thickness is 1.5mm; coating the HIPE emulsion 2 on the upper surface of a non-woven fabric, wherein the thickness is 0.5mm; then the wavelength of 450nm and the intensity of 50mW/cm are adopted 2 And (3) placing the liquid sanitary towel into a steam tunnel furnace for curing for 5min, and dehydrating, drying and cutting to obtain the liquid sanitary towel absorption core.
Fig. 1 is an SEM image of the upper and lower layers of the absorbent core of the liquid sanitary napkin prepared in example 1.
Example 2
A method for preparing an absorbent core of a liquid sanitary napkin, comprising the steps of:
s0. adding dimethylaminoethyl methacrylate, 1-chloroeicosane (dimethylaminoethyl methacrylate: 1-chloroeicosane=1:1, n/n) and a trace amount of polymerization inhibitor (phenothiazine) into acetone, stirring at 45 ℃ for reaction for 20h, centrifuging, washing and drying to obtain a surfactant;
s1, mixing 60 parts of stearyl acrylate, 25 parts of ethylene glycol dimethacrylate, 1 part of a photoinitiator and 8 parts of a surfactant to obtain an oil phase 1, and then adding a water phase A containing 2 mass percent of calcium chloride and a water phase B containing 7 mass percent of an initiator, 0.5 mass percent of sodium acrylate, 0.5 mass percent of sodium methacrylate sulfonate and 0.5 mass percent of sodium acrylate sulfonate, wherein the volume ratio of the oil phase 1 to the water phase A to the water phase B is 1:30:1 to obtain HIPE emulsion 1;
specifically, in the continuous emulsifying device, an oil phase is prepared in an oil phase material storage tank, an inorganic salt water phase is prepared in an aqueous phase material storage tank, an initiator aqueous phase is prepared in an initiator storage tank, when the emulsifying device stably operates, the emulsion part of primary mixing emulsification in a first static mixer module is controlled by a first backflow constant flow pump to be conveyed back to a first emulsifying kettle, and the emulsion part of secondary mixing emulsification in a second static mixer module is controlled by a second backflow constant flow pump to be conveyed back to a second emulsifying kettle; the flow of the reflux is precisely controlled by a first reflux constant flow pump, and meanwhile, the oil phase in an oil phase material storage tank and the water phase in a water phase material storage tank are respectively and continuously conveyed into a first emulsifying kettle through an oil phase feeding constant flow pump and a water phase feeding constant flow pump to be premixed with the emulsion in the kettle which is being mixed and emulsified to obtain a premixed material, and the premixed material is conveyed into a first static mixer module to be mixed and emulsified to obtain a premixed emulsion I with the water-oil ratio of 14:1;
the first premixed emulsion is respectively partially conveyed into a first emulsifying kettle through a first backflow constant flow pump and is conveyed into a second emulsifying kettle through a first premixed emulsion feeding constant flow pump and a control, the first premixed emulsion in the first premixed emulsion feeding constant flow pump and the water phase continuously conveyed into the second emulsifying kettle through the water phase feeding constant flow pump are premixed and combined to obtain a premixed material, and the premixed material is conveyed into a second static mixer module to be mixed and emulsified to obtain a second premixed emulsion; the premixed emulsion II is respectively and partially conveyed into a second emulsifying kettle through a second reflux constant flow pump control, is conveyed to a third static mixer module through a constant flow pump and control, and is finally mixed and emulsified with an initiator water phase which is continuously conveyed through an initiator feeding constant flow pump control, and HIPE emulsion 1 is obtained after mixed and emulsified, and is continuously conveyed to the next procedure through an emulsified product output interface;
s2, mixing 50 parts of isooctyl methacrylate, 20 parts of ethylene glycol dimethacrylate, 1 part of a photoinitiator and 5 parts of the surfactant to obtain an oil phase 2, and then adding a water phase C containing 1% of calcium chloride by mass and a water phase D containing 6% of an initiator by mass, 0.5% of sodium acrylate, 0.5% of sodium methacrylate sulfonate and 0.5% of sodium acrylate sulfonate, wherein the volume ratio of the oil phase 2 to the water phase C to the water phase D is 1:28:1 to obtain HIPE emulsion 2;
the HIPE emulsion 2 was treated in a continuous emulsification apparatus as described in S1;
s3, coating the HIPE emulsion 1 on the lower surface of a non-woven fabric, wherein the thickness is 1.5mm; coating the HIPE emulsion 2 on the upper surface of a non-woven fabric, wherein the thickness is 0.5mm; then the wavelength of 350nm and the intensity of 40mW/cm are adopted 2 And (3) placing the liquid sanitary towel into a steam tunnel furnace for curing for 5min, and dehydrating, drying and cutting to obtain the liquid sanitary towel absorption core.
Example 3
A method for preparing an absorbent core of a liquid sanitary napkin, comprising the steps of:
s0. adding dimethylaminoethyl methacrylate, 1-chlorodocosane (dimethylaminoethyl methacrylate: 1-chlorodocosane=1:1, n/n) and trace polymerization inhibitor (phenothiazine) into acetone, stirring at 40deg.C for reacting for 25h, centrifuging, washing, and drying to obtain surfactant;
s1, mixing 80 parts of eicosanoate, 40 parts of ethylene glycol dimethacrylate, 1 part of a photoinitiator and 8 parts of a surfactant to obtain an oil phase 1, and then adding a water phase A containing 3% of calcium chloride by mass and a water phase B containing 10% of an initiator by mass, 0.4% of sodium acrylate, 0.4% of sodium methacrylate, 0.1% of sodium methacrylate sulfonate and 0.1% of sodium acrylate, wherein the volume ratio of the oil phase 1 to the water phase A to the water phase B is 1:20:1 to obtain HIPE emulsion 1;
specifically, in the continuous emulsifying device, an oil phase is prepared in an oil phase material storage tank, an inorganic salt water phase is prepared in an aqueous phase material storage tank, an initiator aqueous phase is prepared in an initiator storage tank, when the emulsifying device stably operates, the emulsion part of primary mixing emulsification in a first static mixer module is controlled by a first backflow constant flow pump to be conveyed back to a first emulsifying kettle, and the emulsion part of secondary mixing emulsification in a second static mixer module is controlled by a second backflow constant flow pump to be conveyed back to a second emulsifying kettle; the flow of the reflux is precisely controlled by a first reflux constant flow pump, and meanwhile, the oil phase in an oil phase material storage tank and the water phase in a water phase material storage tank are respectively and continuously conveyed into a first emulsifying kettle through an oil phase feeding constant flow pump and a water phase feeding constant flow pump to be premixed with the emulsion in the kettle which is being mixed and emulsified to obtain a premixed material, and the premixed material is conveyed into a first static mixer module to be mixed and emulsified to obtain a premixed emulsion I with the water-oil ratio of 14:1;
the first premixed emulsion is respectively partially conveyed into a first emulsifying kettle through a first backflow constant flow pump and is conveyed into a second emulsifying kettle through a first premixed emulsion feeding constant flow pump and a control, the first premixed emulsion in the first premixed emulsion feeding constant flow pump and the water phase continuously conveyed into the second emulsifying kettle through the water phase feeding constant flow pump are premixed and combined to obtain a premixed material, and the premixed material is conveyed into a second static mixer module to be mixed and emulsified to obtain a second premixed emulsion; the premixed emulsion II is respectively and partially conveyed into a second emulsifying kettle through a second reflux constant flow pump control, is conveyed to a third static mixer module through a constant flow pump and control, and is finally mixed and emulsified with an initiator water phase which is continuously conveyed through an initiator feeding constant flow pump control, and HIPE emulsion 1 is obtained after mixed and emulsified, and is continuously conveyed to the next procedure through an emulsified product output interface;
s2, mixing 60 parts of isooctyl methacrylate, 20 parts of ethylene glycol dimethacrylate, 1 part of a photoinitiator and 2 parts of the surfactant to obtain an oil phase 2, and then adding a water phase C containing 2 mass percent of calcium chloride and a water phase D containing 5 mass percent of the initiator, 0.5 mass percent of sodium acrylate, 0.5 mass percent of sodium methacrylate sulfonate and 0.5 mass percent of sodium acrylate, wherein the volume ratio of the oil phase 2 to the water phase C to the water phase D is 1:40:1 to obtain HIPE emulsion 2;
the HIPE emulsion 2 was treated in a continuous emulsification apparatus as described in S1;
s3, coating the HIPE emulsion 1 on the lower surface of a non-woven fabric, wherein the thickness is 1.5mm; the HI is processedThe PE emulsion 2 is coated on the upper surface of the non-woven fabric, and the thickness is 0.5mm; then the wavelength of 205nm and the intensity of 1000mW/cm are adopted 2 And (3) placing the liquid sanitary towel into a steam tunnel furnace for curing for 5min, and dehydrating, drying and cutting to obtain the liquid sanitary towel absorption core.
Comparative example 1
A method for preparing an absorbent core of a liquid sanitary napkin, the comparative example differs from example 1 in that: in steps S1, S2, the surfactant was replaced with conventional emulsifier propyldimethyl ammonium bromide, and other materials and preparation methods were the same as in example 1.
Comparative example 2
A method for preparing an absorbent core of a liquid sanitary napkin, the comparative example differs from example 1 in that: the 1-chlorobehene in step S0 was replaced with n-butyl chloride, and the eicosane methacrylate in step S1 was replaced with isooctyl methacrylate, and the other materials and preparation methods were the same as in example 1.
Test case
Performance comparison tests were performed on example 1 and comparative examples 1-2.
The testing method comprises the following steps: GB/T14207-2008 was used for water absorption and blood absorption tests.
The test results are shown in Table 1.
TABLE 1 absorption test results
As can be seen from table 1, the specific surfactant and the acrylate monomer are compounded to generate a good synergistic effect in the embodiment 1 of the invention, and the prepared liquid sanitary towel absorbent core has excellent liquid absorption capacity, and the penetration time, rewet amount, water absorption amount and absorption speed are obviously superior to those of the comparative example. In comparative examples 1-2, however, the surfactant was deleted or replaced with a short-chain structure, which resulted in the reaction, and the absorbent core was difficult to form a more three-dimensional, dense microporous structure, and the absorbent capacity of the core was significantly reduced, and no ideal capillary action could be produced, so that the liquid conductivity in the product was poor, and the absorption efficiency was low.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (4)

1. A method for preparing an absorbent core of a liquid sanitary napkin, comprising the steps of:
s1, mixing an acrylic ester monomer 1, a cross-linking agent, a photoinitiator and a surfactant to obtain an oil phase 1, and then adding a water phase A comprising inorganic salt and a water phase B comprising the initiator and acrylic acid salt and/or acrylic sulfonate and derivatives thereof to obtain HIPE emulsion 1;
s2, mixing an acrylic ester monomer 2, a cross-linking agent, a photoinitiator and a surfactant to obtain an oil phase 2, and then adding a water phase C comprising inorganic salt and a water phase D comprising the initiator, acrylic acid salt and/or acrylic sulfonate and derivatives thereof to obtain HIPE emulsion 2;
s3, respectively coating the HIPE emulsion 1 and the HIPE emulsion 2 on the upper surface and the lower surface of cloth, and dehydrating and drying after the treatments of illumination and steam to obtain the liquid sanitary towel absorption core;
wherein,,
the surfactant is obtained by reacting acrylic amino alkyl ester and/or acrylic amino alkyl ester derivative with haloalkane and/or haloalkane derivative;
the inorganic salt is selected from one or more of alkaline earth metal chloride or sulfate and alkali metal chloride or sulfate;
the cloth is selected from one of woven cloth or non-woven cloth;
the acrylic ester monomer 1 is selected from alkyl acrylate or alkyl methacrylate, and the alkyl in the alkyl acrylate or alkyl methacrylate is selected from C18-C20 alkyl;
the acrylic ester monomer 2 is selected from isooctyl acrylate or isooctyl methacrylate;
the preparation method of the surfactant comprises the following steps:
adding acrylic amino alkyl ester and/or acrylic amino alkyl ester derivative, alkyl halide and/or alkyl halide derivative and polymerization inhibitor into solvent, heating and stirring at 40-60 ℃ for reaction, and purifying to obtain the surfactant;
in the haloalkane and/or haloalkane derivative, halogen atoms are selected from one of fluorine atoms, chlorine atoms, bromine atoms and iodine atoms; the carbon number of the alkyl is selected from 20-22;
in the step S1, the mass ratio of the acrylic ester monomer 1 to the cross-linking agent to the photoinitiator to the surfactant is (40-100): 5-40): 0.05-2): 2-10; in the water phase A, the mass fraction of inorganic salt is 1-4%; in the water phase B, the mass fraction of the initiator is 0.1-10%, and the mass fraction of the acrylate and/or the acrylate sulfonate and the derivative thereof is 0.1-5%; the volume ratio of the oil phase 1 to the water phase A to the water phase B is 1 (20-40): 1-10;
in the step S2, the mass ratio of the acrylic ester monomer 2 to the cross-linking agent to the photoinitiator to the surfactant is (40-100): 5-40): 0.05-2): 2-10; in the water phase C, the mass fraction of the inorganic salt is 1-4%; in the water phase D, the mass fraction of the initiator is 0.1-10%, and the mass fraction of the acrylate and/or the acrylate sulfonate and the derivative thereof is 0.1-5%; the volume ratio of the oil phase 2 to the water phase C to the water phase D is 1 (28-40): 1-10;
in step S3, the light has a wavelength of 205-450nm and an intensity of 40-1000mW/cm 2 The time is 5-180 and s.
2. A method of preparing a liquid sanitary napkin absorbent core according to claim 1, wherein the alkyl groups in the alkyl esters are selected from C1-C20 alkyl groups in the aminoalkyl acrylate and/or aminoalkyl acrylate derivatives; the amino group is-N (R) 1 )(R 2 ) The R is 1 And R is 2 Independently selected from a hydrogen atom or a C1-C20 alkyl group;
in the amino alkyl acrylate derivative,
one or more hydrogen atoms on the acrylic group are substituted with one or more of a fluorine atom, a chlorine atom, a bromine atom, an iodine atom, or a C1-C20 alkyl group;
and/or the number of the groups of groups,
one or more carbon atoms in the alkyl group are replaced by one or more of polyethylene glycol, polypropylene glycol and polytetramethylene glycol chain segments;
and/or the number of the groups of groups,
the c=c double bond on the acrylic group can be reduced, oxidized or added to a different group.
3. The method of making a liquid sanitary napkin absorbent core according to claim 1 wherein said HIPE emulsion 1 and HIPE emulsion 2 are made using a continuous emulsifying apparatus.
4. The method of preparing a liquid sanitary napkin absorbent core according to claim 1, wherein the cross-linking agent is selected from one or more of ethylene glycol diacrylate, ethylene glycol dimethacrylate, butylene glycol diacrylate, hexylene glycol dimethacrylate, trimethylol triacrylate, tripropylene glycol diacrylate, trimethylol trimethacrylate, tripropylene glycol dimethacrylate.
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CN108084330A (en) * 2017-12-27 2018-05-29 佛山市飞吸高分子材料科技有限公司 A kind of esters of acrylic acid porous polymer and preparation method thereof
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CN114410045A (en) * 2022-03-09 2022-04-29 万华化学集团股份有限公司 Method for preparing bacteriostatic foam absorbing material from HIPPE, foam absorbing material and application thereof

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CN1140458A (en) * 1994-12-08 1997-01-15 株式会社日本触媒 Water-absorbent resin, process for production thereof, and water-absorbent resin composition
CN108084330A (en) * 2017-12-27 2018-05-29 佛山市飞吸高分子材料科技有限公司 A kind of esters of acrylic acid porous polymer and preparation method thereof
CN113289049A (en) * 2021-05-28 2021-08-24 广州安洁芯材科技有限公司 Preparation method of acrylic foam material absorption core
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