CN107501462A - A kind of bacteriostasis, and deodorization super absorbent resin and the absorbent article containing the super absorbent resin - Google Patents

A kind of bacteriostasis, and deodorization super absorbent resin and the absorbent article containing the super absorbent resin Download PDF

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Publication number
CN107501462A
CN107501462A CN201710671956.8A CN201710671956A CN107501462A CN 107501462 A CN107501462 A CN 107501462A CN 201710671956 A CN201710671956 A CN 201710671956A CN 107501462 A CN107501462 A CN 107501462A
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absorbent resin
super absorbent
bacteriostasis
deodorization
parts
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洪锡全
裴小苏
周丕严
刘若铎
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Zhejiang Satellite Mstar Technology Ltd
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Zhejiang Satellite Mstar Technology Ltd
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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
    • 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
    • A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
    • 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
    • A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
    • 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
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/28—Polysaccharides or their derivatives
    • 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
    • A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
    • 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
    • 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
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/245—Differential crosslinking of one polymer with one crosslinking type, e.g. surface crosslinking
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0091—Complexes with metal-heteroatom-bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions 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
    • C08L33/02—Homopolymers or copolymers of acids; Metal or ammonium salts 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104—Silver, e.g. silver sulfadiazine
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    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2333/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
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Abstract

The present invention provides a kind of bacteriostasis, and deodorization super absorbent resin, in the mixed liquor of the acrylic acid/acrylates formed in by alkali formula compound with acrylic monomers solution, add just crosslinking agent, the first dispersant and antiseptic being stirring evenly and then adding into continues to stir, it is warming up to 35 DEG C 70 DEG C and adds the colloidal super absorbent resin that initiator is polymerized, granulation is passed sequentially through to the colloidal super absorbent resin, dry, and core-shell type super absorbent resin of the acquisition with three-dimensional crosslinked network structure for being surface-treated and being formed using composite antibacterial crosslinking agent at a temperature of 110 180 DEG C.The antiseptic is one or both of amino acid metal salt ion chelate complex, chitin metal salt ion chelate complex composition.The present invention is applied to sanitary absorbent article, and bacteriostasis, and deodorization performance is notable, and raw material is easy to get, and cost is cheap, has huge benefit.

Description

A kind of bacteriostasis, and deodorization super absorbent resin and the absorbent article containing the super absorbent resin
Technical field
The invention belongs to the research field of feature super absorbent resin, more particularly to a kind of bacteriostasis, and deodorization high-hydroscopicity tree Fat and its absorbent article using bacteriostasis, and deodorization super absorbent resin.
Background technology
Super absorbent resin (super absorbent polymer, SAP) is with higher water absorption energy and water retention property High molecular polymer general name.Abroad, in the early 1950s, Goodrich companies of the U.S. develop cross linked polyacrylate Resin, subsequent United States Department of Agriculture north research center Russell et al. set about studying the grafting of starch and acrylonitrile in 1961 Technology；By 1978, SANYO GS chemical conversion company researches and develops and industrialization production starch graft polyacrylate copoly type high water absorption Property resin.At home, super absorbent resin research is started in the early 1980s, due to starting evening, the visitor such as development time is short Sight factor, the super absorbent resin innovation ability and technology development capability of China's production all can not be compared with foreign countries.
Originally, super absorbent resin is mainly as water-loss reducer, extensively using then agricultural technology field, with high-hydroscopicity Resin starts to the demand of super absorbent resin both at home and abroad as a large amount of uses of the carrier in disposable sanitary articles are absorbed Drastically expand, average annual growth rate is up to 30%~40%, to grinding for kind, route of synthesis, performance and application field etc. Study carefully and reach its maturity.
Different according to the raw material sources of super absorbent resin, super absorbent resin is broadly divided into three big series：Starch-series, fiber Prime system, synthesis system, wherein the polyacrylate in synthesis system is due to original abundance, cheap, long-term preservation, synthesis The features such as water absorbing properties are excellent as current research emphasis.
Superabsorbent polyacrylate resin in synthesis system causes with good absorbent properties, as absorbing medium It is widely used in disposable sanitary articles, therefore, the domestic research to polyacrylie-type super absorbent resin at present It is all based on the research of its application performance in disposable hygienic product, including low monomer residue amount technology, pressure-resistant water absorption rate, height Fast rate of water absorption and anti-caking performance etc., still, antibacterial and deodoriging properties to superabsorbent polyacrylate resin Study less.
It is total well known, the urine complicated of people, mainly contain urea and various inorganic ions, such as Na+、Cl-、K+、 SO4 2-Deng the urine of people is converted into the smell for not arriving unpleasant ammonia in the presence of various microorganisms, for the people of Long-term taking medicine For, its urine taste is even more serious, is particularly easy to cause disease at heart and various disease of skin, such as erythema.It is general to overcome Existing above mentioned problem, industry technology expert, technical staff are anti-in effort research in use for logical super absorbent resin The super absorbent resin of bacterium property or bacteriostasis, and deodorization.
In known technology field, the patent of invention of Application No. 201310560034.1 discloses a kind of Tea Polyphenols-propylene Acid system super absorbent resin, it is first to neutralize acrylic acid with sodium hydroxide solution, then with N, N '-methylene-bisacrylamide For crosslinking agent, potassium peroxydisulfate is initiator, occurs polymerisation with Tea Polyphenols in water, reacted gel through cooling down, shearing, It is dry and manufactured.
However, the reinforcement with health perception with the improvement of people ' s living standards, antibacterial product has become people's life In an indispensable part, because silver ion is safe and non-toxic to human body cell and immune system, and anti-microbial property is splendid, so Inorganic resistance agent is prepared usually using silver ion and its compound, current silver-based inorganic antibacterial agent is extensively using then chemical fibre, modeling The every field such as material products, building materials, glass, ceramics, coating, water process and cosmetics.Metal ion with antibacterial activity has Silver, chromium, cobalt, nickel, aluminium, copper, zinc, iron plasma, consider, Ag jointly from security and antibiotic property+Preferably, Zn2+Take second place, therefore, Silver ion antimicrobial agent occupies leading position in inorganic antiseptic.
The patent of invention of Application No. 201410175092.7 discloses a kind of antibacterial high water-absorbent resin and its preparation Method, the resin are a kind of functional high molecule materials, and carboxylic acid group and institute's acid are contained on long-chain, side chain containing allylic structure Sodium, there is internally crosslinked porous type network structure, particle is internal or external to contain solubilising quaternary ammonium salt cationic monomer, adopts Prepared with redox initiation system water solution polymerization process, the oxidant used is for sodium peroxydisulfate or ammonium persulfate, reducing agent Sodium sulfite or sodium hydrogensulfite, crosslinking agent N, N '-methylene-bisacrylamide or polyethyleneglycol diacrylate.
The patent of invention of Application No. 201410682192.9 discloses a kind of preparation side of natural antibacterial water-absorbing resin Method, this method are under the conditions of ice-water bath, with alkali lye and acrylic acid solution, then sequentially adding acrylamide, natural poly- electricity Mass shell glycan, crosslinking agent and initiator are solved, is stirred, then in 70-90 DEG C of reaction, after gel occurs in system, is continued anti- Answer and be incubated 1 hour under temperature conditionss, produce natural high antibiotic property super absorbent resin.
The patent of invention of Application No. 201410658347.5 discloses a kind of preparation method of antibiotic property high hydroscopic resin, Add acrylic acid, deionized water in the reactor first, add 50% sodium hydroxide solution and neutralize, addition acryloyl morpholine, Superfine silicon dioxide and multiple crosslinking agent, then with nitrogen deoxygenation 30min, add initiator and trigger polymerization to harden at 20-30 DEG C, Temperature, which no longer rises, to be considered as reaction and terminates, by colloid through being granulated, drying, broken obtain water absorbing resin particle, last resin particle Through ethylene glycol, produce after 120 DEG C of high-temperature process 2-5 hours of nano silver antimicrobials and 25% aluminum sulfate.
Notification number is that CN104403249B patent of invention discloses a kind of preparation method of antibiotic property high hydroscopic resin, should Preparation method adds acrylic acid, deionized water in the reactor first, adds 50% sodium hydroxide solution neutralization, adds propylene Acyl group morpholine, superfine silicon dioxide and multiple crosslinking agent, then lead to nitrogen deoxygenation 30min, add initiator in 20-30 DEG C of initiation Polymerisation, temperature, which no longer rises, to be considered as reaction and terminates, by colloid through being granulated, drying, broken obtain water absorbing resin particle；Finally Resin particle produces product through ethylene glycol, nano silver antimicrobials and 25% aluminum sulfate after 120 DEG C of high-temperature process 2-5 hours, because Its surface employs nano silver antimicrobials processing so that resin particle has good antibacterial, bactericidal effect.
Notification number is that CN103992425A patent of invention discloses a kind of antibacterial high water-absorbent resin and its preparation side Method, the resin are a kind of functional high molecule materials, and carboxylic acid group and carboxylic acid are contained on long-chain, side chain containing allylic structure Sodium, there is internally crosslinked porous network structure, particle is internal or external to contain solubilising quaternary ammonium salt cationic monomer, adopts Prepared with redox initiation system water solution polymerization process, oxidant is sodium peroxydisulfate or ammonium persulfate, and reducing agent is sulfurous acid Sodium or sodium hydrogensulfite, crosslinking agent N, N '-methylene-bisacrylamide or polyethyleneglycol diacrylate, the high water absorption of preparation Property resin there is good suction water retention property, logical fluidity energy and high rate of liquid aspiration, wherein added solubilising quaternary ammonium salt sun from Sub- property monomer causes super absorbent resin to have preferable anti-microbial property.
In addition, chitosan is unique a large amount of existing basic amine group polysaccharide in natural polysaccharide, there is good bio-compatible The performances such as the antibiotic property of property, biological degradability and wide spectrum, these performances make it as natural antibiotic antiseptic, anti-biotic material, Application prospect in fields such as medical treatment, food, cosmetics is very wide.
Known technology in the art is made a general survey of, it mainly reaches anti-by adding nano-silver ionic or quaternary ammonium salt ion The effect of bacterium, but the above method is applied in the personal commodity of women and children except larger potential safety hazard be present, to user's Outside body may damage, directly using Ag+ as antibacterial ion, following defect also be present：(1) Ag+ is easily reduced into list Matter is silver-colored and is changed into black, influences application of the silver ion antimicrobial agent in light color article, anti-tarnishing ability is poor；(2) in alkaline environment In easily generation Ag2O precipitation, sustained release performance is poor, influences Durability of antimicrobial effect；(3) when Ag+ meets Cl- article or environment, easily generation AgCl precipitations be silver-colored deposited phenomenon cause its anti-microbial property substantially weaken in addition fail, salt resistant character is poor, (4) silver carrying amount compared with Low, antibacterial effect is limited.
Based on technical problem present in prior art, the present invention provides comprising amino acid, chitosan chelated nano silver, received Bacteriostasis, and deodorization super absorbent resin of chelate antiseptic of rice zinc and preparation method thereof, there is provided one kind has sustained-release antibacterial function Super absorbent resin, solve existing metal ion particularly silver ion antimicrobial agent is easy to change, sustained release performance and salt tolerance are poor, The technical problems such as silver carrying amount is low,
The content of the invention
It is an object of the invention to provide a kind of bacteriostasis, and deodorization super absorbent resin so that super absorbent resin keeps high water absorption While multiplying power, high water conservation multiplying power, high-selenium corn speed, high withstand voltage performance, it is safe, comfortable, health care to assign women and children user Product.
In order to realize above-mentioned target, a kind of natural high bacteriostasis, and deodorization super absorbent resin of the invention, used skill Art scheme is：Described bacteriostasis, and deodorization super absorbent resin, it is with the superabsorbent polyacrylate with certain degree of cross linking Resin is matrix resin, is combined with antimicrobial composition between the network molecule chain in the super absorbent resin, or/and Antimicrobial composition is loaded with the three-dimensional crosslinked network structure on super absorbent resin surface, for suppressing super absorbent resin glue Body breed bacteria and peculiar smell, the antimicrobial composition are amino acid metal salt ion chelate complex, chitosan-metal salt ion chela One or both of compound forms.The super absorbent resin be through deionized water dilute and by alkali formula compound in and third In the mixed liquor for acrylic acid/acrylates that acrylic monomer solution forms, just crosslinking agent, first dispersant and after stirring are added The antimicrobial composition for adding 0-80% continues to stir, and is warming up to 35 DEG C -70 DEG C and adds the colloid that initiator is polymerized Shape super absorbent resin, granulation is passed sequentially through to the colloidal super absorbent resin, is dried, and adopted at a temperature of 110-180 DEG C With what is mainly formed by the rear dispersant configuration of multiple crosslinking agent and 20%-100% resistance agent composition and 0.05-3 parts Polyacrylate shell core of the acquisition with three-dimensional crosslinked network structure that composite antibacterial crosslinking agent is surface-treated and formed Type super absorbent resin, is counted in parts by weight, the antimicrobial composition of monomer 0.05-50 parts in 100 parts of acrylic acid.
Preferably, the composite antibacterial crosslinking agent by 20%-100% antiseptic and described multiple crosslinking agent, after Dispersant, deionized water configuration form, and the concentration of composite antibacterial crosslinking agent is 5%-50% solution, 30-45 DEG C of solution temperature.
Preferably, the antimicrobial composition compositing formula also includes nano inorganic powder and coupling agent, by weight Number meter, nano inorganic powder is 0.1-30 parts；The addition of the coupling agent is the 0.5%- of nano inorganic powder parts by weight 3.5%；It is 30%-70%'s that 20%-100% antiseptic is configured to concentration by the composite antibacterial crosslinking agent with deionized water Solution, nano inorganic powder is added after being warming up to 30-50 DEG C, stirring and ultrasonic wave disperse 10-20min, make antiseptic uniformly solid The particle surface of nano inorganic powder is scheduled on, filtered after standing 30-60min, obtain antimicrobial nano inorganic particle after vacuum drying, And surface coupling processing is carried out to antibacterial nano inorganic powder and obtains antimicrobial nano inorganic particle, then will be compound with deionized water Crosslinking agent is configured to the solution that concentration is 5%-50%, and is warming up to 30-45 DEG C, then by the antimicrobial nano inorganic particle, rear point Powder is added and stirred, and is continued ultrasonic wave 10-20min and divided equally the scattered heat treatment crosslinked fluid formed.
The amino acids metal ion chelate complex includes amino acid nano-silver ion chelate complex, amino acid nanometer zinc ion chela Compound；The chitin metal salt ion chelate complex includes chitosan nano silver ion chelate complex, chitosan nano zinc ion chela Compound.
One kind after described in dispersant selection polyvinyl alcohol, hydroxymethyl cellulose, sodium pyrophosphate, sodium pyrophosphate decahydrate；
The present invention provides a kind of preparation method of super absorbent resin, and it is counted in parts by weight, the super absorbent resin Composition and parts by weight it is as follows：
100 parts of acrylic acid；
Alkali formula compound 35-45 parts；
Deionized water 105-145 parts；
First crosslinking agent 0.006-1.8 parts；
Initiator 0.005-2 parts；
First dispersant 0.005-4 parts；
Multiple crosslinking agent 0.3-4 parts.
The preparation method of bacteriostasis, and deodorization super absorbent resin of the present invention, including emulsion polymerization, reverse (reverse) Suspension polymerization, mass polymerization and water solution polymerization process, the preparation method are preferably water solution polymerization process, and the aqueous solution gathers Legal preparation process comprises the following steps：
1) the step of acid-base neutralization：By after 100 parts of refined acrylic monomers mix with the deionized water of 105-145 parts The alkali formula compound for adding 35-45 parts is neutralized, and degree of neutralization is 60%~85%, and acrylic acid and acrylic acid are obtained after neutralization The quality total concentration of sodium is 30%~60% mixed liquor M1.
2) the step of polymerization is triggered：Added into mixed liquor M1 the first crosslinking agent of 0.006-1.8 parts, 0.005-4 parts just The 0-80% of dispersant and antiseptic number, stirs or sonic oscillation 12-25min forms mixed liquor M2, will mix Liquid M2 is gradually heating to 35 DEG C~70 DEG C, and the initiator for then adding 0.005-2 parts carries out polymerisation 30s~3min, obtains Gelatinous polymer.
3) the step of being granulated：Gelatinous polymer obtained by step (2) is granulated, is placed in 85 DEG C~158 DEG C of temperature The lower drying 6min~58min of degree, obtains granulated polymer.
4) the step of multiple crosslinking agent：This step includes antiseptic pretreatment and obtains the antimicrobial nano through surface coupling processing The step of inorganic particle, the multiple crosslinking agent of 0.3-4 parts is configured to the solution M4 that concentration is 5%-50% with deionized water, and 30-45 DEG C is warming up to, antimicrobial nano inorganic particle, the rear dispersant of 0.05-3 parts of step (4) processing are added in solution M4 Stir, and continue to disperse 10-20min acquisition heat treatment crosslinked fluids M5 using ultrasonic wave.
5) surface-crosslinked step：Heat treatment crosslinked fluid M5 is used into spray-on process to gained at a temperature of 110-180 DEG C Granular polymer carry out heat cross-linking surface treatment, be stirred mixing and heat drying after obtain there is three-dimensional crosslinked network structure Core-shell type super absorbent resin.
Further, the step of antiseptic pre-processes is as follows：Surplus antiseptic is configured into concentration with deionized water is 30%-70% solution M3, and 30-50 DEG C is warming up to, the nano inorganic powder stirring that 0.1-30 parts are added in solution M3 is equal It is even, and continue to disperse 10-20min using ultrasonic wave, antiseptic is fixed on to the particle surface of nano inorganic powder, stands 30- Filtered after 60min, obtain antimicrobial nano inorganic particle after vacuum drying, antimicrobial nano inorganic particle is then placed in high-speed kneading In machine, then add the coupling agent that addition is nano inorganic powder parts by weight 0.5%-3.5% and carry out high speed surface coupling Cladding processing.
The antiseptic is amino acid metal salt ion chelate complex, one kind in chitin metal salt ion chelate complex or two Kind composition.
As further preferably, metal ion of the present invention is the metal ion for having antibacterial activity, is included Silver, chromium, cobalt, nickel, aluminium, copper, zinc, iron plasma, consider, preferably Ag jointly from security and antibiotic property+、Zn2+, the amino acid Chelate of metal ion includes amino acid nano-silver ion chelate complex, amino acid Nano-Zinc ion chelate complex.The chitosan gold Belonging to salt ion chelate includes chitosan nano silver ion chelate complex, chitosan nano Zinc Ions Chelated thing.As further Preferred scheme, the antiseptic also includes Tea Polyphenols, carboxymethyl chitosan or carboxymethyl chitosan quaternary ammonium salt, in parts by weight Meter, the Tea Polyphenols addition is 1-30 parts, and the carboxymethyl chitosan quaternary ammonium salt is calculated by weight as 1-40 parts.
As it is further preferably, the just crosslinking agent is N, N '-methylene-bisacrylamide, polyethylene glycol 200, fourth two One kind in alcohol, pentaerythrite, Pehanorm triacrylate.
As further preferably, the multiple crosslinking agent is ethers, esters, handed over containing two and two or more hydroxy alcohols Join wherein at least a kind of composition in agent.
As further preferably, the ethers crosslinking agent uses polyethyleneglycol diglycidylether, the esters crosslinking Agent is using one or both of polyethylene glycol 200 diacrylate, Pehanorm triacrylate, the alcohols crosslinking Agent is that the wherein at least one in polyethylene glycol 200, butanediol, pentaerythrite is formed.
As further preferably, the just dispersant is selected in polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone It is a kind of；One kind after described in dispersant selection polyvinyl alcohol, hydroxymethyl cellulose, sodium pyrophosphate, sodium pyrophosphate decahydrate.
Preferably the initiator be redox initiation system as further, and reducing agent is bisulfites, it is different to resist The bad one of which learned in hydrochlorate；Oxidant is selected from the one of which in persulfate, hydrogen peroxide；Alkali formula compound is chosen One of which in sodium hydroxide, potassium hydroxide.
As it is further preferably, the nano inorganic powder is nano silicon, nano titanium oxide, nano oxidized One or both of aluminium combines, and the nano silicon, nano titanium oxide, the particle diameter of nano aluminium oxide are 10-50nm.
In some possible embodiments, antiseptic is not added in the step of initiation polymerization of abovementioned steps (2), and Antiseptic is made an addition in the antiseptic pre-treatment step of abovementioned steps (4).
In other possible embodiments, antiseptic is not added in the step of initiation polymerization of abovementioned steps (2), And directly antiseptic is made an addition in the solution of multiple crosslinking agent of surface treatment stage, while by key element nano inorganic powder and Coupling agent omits, and its preparation process includes as follows：
1) the step of acid-base neutralization：By after 100 parts of refined acrylic monomers mix with the deionized water of 105-145 parts The alkali formula compound for adding 35-45 parts is neutralized, and degree of neutralization is 60%~85%, and acrylic acid and acrylic acid are obtained after neutralization The quality total concentration of sodium is 30%~60% mixed liquor M1.
2) the step of polymerization is triggered：Added into mixed liquor M1 the first crosslinking agent of 0.006-1.8 parts, 0.005-4 parts just The 0-80% of dispersant and antiseptic number, stirs or sonic oscillation 12-25min forms mixed liquor M2, will mix Liquid M2 is gradually heating to 35 DEG C~70 DEG C, and the initiator for then adding 0.005-2 parts carries out polymerisation 30s~3min, obtains Gelatinous polymer.
3) the step of being granulated：Gelatinous polymer obtained by step (2) is granulated, is placed in 85 DEG C~158 DEG C of temperature The lower drying 6min~58min of degree, obtains granulated polymer.
4) the step of composite antibacterial crosslinking agent：The multiple crosslinking agent of 0.3-4 parts is configured into concentration with deionized water is 5%-50% solution M4, and 30-45 DEG C is warming up to, the rear dispersant that 0.05-3 parts are added in solution stirs, then 20%-100% antiseptic is continuously added, and continues to disperse 10-20min acquisition heat treatment crosslinked fluids M5 using ultrasonic wave.
5) surface-crosslinked step：Finally, this heat treatment crosslinked fluid M5 is used into spray-on process pair at a temperature of 110-180 DEG C Granulated polymer carries out heat cross-linking surface treatment obtained by step (3), is obtained after being stirred mixing and heat drying with three Tie up the core-shell type super absorbent resin of cross-linked network structure.
Application of the foregoing bacteriostasis, and deodorization super absorbent resin in medical treatment, disposable absorbent article, wherein, it is described Disposable absorbent article include baby paper diaper, baby diaper, adult diaper, adult nappy, sanitary napkin, sanitary belt, Pet pads, but preceding feature can not be considered as the limitation for forming application field of the present invention, and such as it is also possible to apply the invention to for kitchen use Paper, blotting paper.
The present invention also provides a kind of absorbent article using foregoing bacteriostasis, and deodorization super absorbent resin, includes transparent liquid Property surface layer, opaque liquid bottom and the absorptive core between liquid permeability surface layer and opaque liquid bottom, it is characterised in that Bacteriostasis, and deodorization super absorbent resin of the present invention is combined with the absorptive core.
Further, the absorptive core includes composite absorption core body, Time of Fluff Slurry absorptive core.Wherein, Time of Fluff Slurry absorbs Core body is the absorptive core mixed by scroll pile pulp fibres, bacteriostasis, and deodorization super absorbent resin.Wherein, the absorbent cores Body is preferably composite absorption core body, and the composite absorption core body includes loft nonwoven layer of cloth, the loft nonwoven layer of cloth be with Height curling hot-melt fiber, or pass through built-up fluffy of interspersed winding with high curling hot-melt fiber, scroll pile pulp fibres Loose network of fibers, upper epidermis, layer in loft nonwoven layer of cloth lay bacteriostasis, and deodorization super absorbent resin respectively, in formation Absorbed layer, lower absorbed layer, the bacteriostasis, and deodorization super absorbent resin in upper absorbed layer, lower absorbed layer are implanted into fluffy fiber net respectively In the upper epidermis of network, the fiber mesh of layer, upper absorbed layer, lower absorbed layer and loft nonwoven layer of cloth are connected as a single entity, together When upper absorbed layer, lower absorbed layer extexine on glued connection top layer coating, bottom coating respectively.
The beneficial effect that the present invention realizes：The present invention has lasting, excellent and sustained release antibacterial effect, not only with compatible Property it is good, safe, to contact no skin irritation the advantages that, and with excellent antibacterial, deodorizing effect, to large intestine bar The bacteriums such as bacterium, staphylococcus aureus, candida albicans have significant inhibitory action, include the medical supplies or once of the present invention Sex hygiene articles for use, user can be allowed to wear comfortable, erythema, the skin scabies for avoiding conventional absorbent paper super absorbent resin from bringing Itch, the safety problem such as peculiar smell, meanwhile, the present invention maintains excellent water absorbing properties, i.e., present invention imparting super absorbent resin is excellent While different bacteriostasis, and deodorization performance, every absorbent properties of super absorbent resin are not influenceed.Raw material of the present invention is easy to get, and cost is low It is honest and clean, significant effect, there is huge economic benefit, social benefit and environmental benefit.
Embodiment
Metal ion such as silver, chromium, cobalt, nickel, aluminium, copper, zinc, iron plasma have anti-microbial property, but due to metal ion sheet Body chemical property is unstable, is easy to be reduced to metal or causes to implement its resistance effect, such as Nano Silver as metal oxide Although ion with excellent anti-microbial property, its because silver ion is not sufficiently stable, be readily converted into argent or silver oxide and Discoloration is produced, its antibacterial ability is seriously reduced, limits its antibacterial effect and application field to a certain extent.Thus may be used See, with the complex ion alternative metals ion of metal ion such as silver ion or zinc ion be solve metal ion be easily oxidised or The most effective approach of reduction, the stability of metal ion is improved by coordination.Because coordination ion has good sustained release Effect, so that metal ion has efficient, the lasting, effect of broad-spectrum antiseptic.
The present invention by will in amino acid, chitosan or carboxymethyl chitosan have strong electronegativity O atom and N atoms, Easily form stronger coordination with metal ion, so as to formed stable metal ion-amino-acid chelate, metal ion- Chitosan Chelate or metal ion-carboxymethyl chitosan chelate, overcome metal antibacterial ion present in prior art The problem of unstable.Consider jointly as the preferred embodiments of the invention, and from security and antibiotic property, metal of the invention The preferred Ag of ion+、Zn2+.Therefore, the amino acids metal ion chelate complex includes amino acid nano-silver ion chelate complex, amino Sour Nano-Zinc ion chelate complex.The chitin metal salt ion chelate complex includes chitosan nano silver ion chelate complex, shell gathers Sugared Nano-Zinc ion chelate complex.As further preferred scheme, the antiseptic also includes Tea Polyphenols, carboxymethyl chitosan Or carboxymethyl chitosan quaternary ammonium salt.Wherein, quaternary ammonium salt is called quarternary ammonium salt, is that four hydrogen atoms in ammonium ion are all taken by alkyl Generation and the compound generated, general formula R 4NX, wherein four alkyl R can be with identical, also can be different.X mostly be halogen anion (F, Cl, Br, I) or acid group (such as HSO, RCOO).
Bacteriostasis, and deodorization super absorbent resin of the present invention, inhaled so that the polyacrylate with certain degree of cross linking is high Water-base resin is matrix resin, in Ke He mechanisms, wherein, stratum nucleare is to be in by first crosslinking agent and polyacrylic acid, polyacrylic acid salinity The polyacrylate polymer with network molecule chain to be formed is crosslinked by low crosslinking degree between subchain, shell is by multiple Crosslinking agent is closed to be crosslinked and the three-dimensional crosslinked network structure of formation, the height by high-crosslinking-degree with polyacrylic acid, polyacrylate Antimicrobial composition, or/and the three-dimensional on super absorbent resin surface are combined between network molecule chain in water-absorbing resins Antimicrobial composition is loaded with cross-linked network structure, the antimicrobial composition is carried on three-dimensional crosslinked network structure and polypropylene On interface between Barbiturates polymer, three-dimensional crosslinked network inside configuration, or/and the extexine of three-dimensional crosslinked network structure, For suppressing high-hydroscopicity matrix resin colloid breed bacteria and peculiar smell.
The bacteriostasis, and deodorization super absorbent resin of the present invention is counted in parts by weight, and its compositing formula and parts by weight are as follows：
100 parts of acrylic acid；Alkali formula compound 35-45 parts；Deionized water 105-145 parts；First crosslinking agent 0.006-1.8 parts； Initiator 0.005-2 parts；First dispersant 0.005-4 parts；Multiple crosslinking agent 0.3-4 parts；；Antiseptic 0.05-50 parts.Enter at some In the preferred embodiment of one step, in addition to rear dispersant 0.05-3 parts nano inorganic powder 0.1-30 parts and coupling agent, institute The addition for stating coupling agent is the 0.5%-3.5% of nano inorganic powder parts by weight.
The antiseptic is preferably 1-10 parts, and nano inorganic powder is preferably 5-15 parts.Wherein, the antiseptic is amino One or both of acid metal salt ion chelate complex, chitin metal salt ion chelate complex form.The amino acids metal from Sub- chelate preferred amino acid nano-silver ionic chelate, amino acid Nano-Zinc ion chelate complex.The chitin metal salt from The preferred chitosan nano silver ion chelate complex of sub- chelate, chitosan nano Zinc Ions Chelated thing.
The preparation method of bacteriostasis, and deodorization super absorbent resin of the present invention, including emulsion polymerization, reverse (reverse) Suspension polymerization, mass polymerization and water solution polymerization process, the preparation method are preferably water solution polymerization process, and the aqueous solution gathers Legal preparation process comprises the following steps：Super absorbent resin of the present invention is being diluted and by alkali formula through deionized water In the mixed liquor of the acrylic acid/acrylates formed in compound with acrylic monomers solution, just crosslinking agent, first dispersant are added And the antiseptic for being stirring evenly and then adding into 0-80% continues to stir, it is warming up to 35 DEG C of -70 DEG C of addition initiators and is polymerized Colloidal super absorbent resin, granulation is passed sequentially through to the colloidal super absorbent resin, is dried, and in 110-180 DEG C of temperature The lower acquisition for being surface-treated and being formed using composite antibacterial crosslinking agent of degree has the core-shell type of three-dimensional crosslinked network structure high Water-absorbing resins.Wherein：
In some preferred embodiments, the composite antibacterial crosslinking agent by 20%-100% antiseptic deionization Water is configured to the solution that concentration is 30%-70%, and nano inorganic powder, stirring and ultrasonic wavelength-division are added after being warming up to 30-50 DEG C 10-20min is dissipated, antiseptic is uniformly fixed on the particle surface of nano inorganic powder, is filtered after standing 30-60min, vacuum is done Antimicrobial nano inorganic particle is obtained after dry, and it is inorganic to obtain antimicrobial nano to antibacterial nano inorganic powder progress surface coupling processing Powder, multiple crosslinking agent is then configured to the solution that concentration is 5%-50% with deionized water, and is warming up to 30-45 DEG C, then The antimicrobial nano inorganic particle, rear dispersant are added and stirred, and continue ultrasonic wave 10-20min, obtains heat treatment crosslinking Liquid.
In other feasible embodiments, antiseptic and institute of the composite antibacterial crosslinking agent by 20%-100% Dispersant, deionized water configuration form after the multiple crosslinking agent stated, and the concentration of composite antibacterial crosslinking agent is 5%-50% solution, 30-45 DEG C of solution temperature.
Alternatively, Tea Polyphenols has anti-oxidant, anti-mutation and the multiple efficacies such as antibacterial.Removed based on the excellent antibacterial of Tea Polyphenols Smelly function, super absorbent resin is made an addition to using Tea Polyphenols as pure natural functional additive, it is excellent to assign super absorbent resin Antibacterial and deodouring function.Therefore, antiseptic of the present invention also includes Tea Polyphenols or carboxymethyl chitosan quaternary ammonium salt, offers tea more Phenol or carboxymethyl chitosan quaternary ammonium salt and amino acid nano-silver ion chelate complex, amino acid Nano-Zinc ion chelate complex, chitosan Nano-silver ionic chelate or chitosan nano Zinc Ions Chelated thing, by the synergy of variety classes antiseptic, further Improve the antibacterial effect of invention.Count in parts by weight, the Tea Polyphenols addition is 1-30 parts, the carboxymethyl chitosan quaternary ammonium Salt is calculated by weight as 1-40 parts.Alternatively, it can also add and citric acid 1- is added in the mixed liquor of acrylic acid/acrylates 10 parts.
Just crosslinking agent of the present invention is N, N '-methylene-bisacrylamide, polyethylene glycol 200, butanediol, Ji Wusi One kind in alcohol, Pehanorm triacrylate, as further preferred embodiment, first crosslinking agent is preferably N, N '-methylene-bisacrylamide.
Multiple crosslinking agent of the present invention is ethers, esters, containing in two and two or more hydroxy alcohols crosslinking agent It is wherein at least a kind of to form.Wherein, the ethers crosslinking agent uses polyethyleneglycol diglycidylether, and the esters crosslinking agent is adopted With one or both of polyethylene glycol 200 diacrylate, Pehanorm triacrylate, the crosslinkers are Wherein at least one in polyethylene glycol 200, butanediol, pentaerythrite is formed.It is described as further preferably square implementation case Multiple crosslinking agent is preferably polyethyleneglycol diglycidylether, polyethylene glycol 200 by 1:The compound friendship that the configuration of 1 mol ratio forms Join agent, or polyethyleneglycol diglycidylether, pentaerythrite press 1:The multiple crosslinking agent that the configuration of 1 mol ratio forms.
The just dispersant of the present invention selects one kind in polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, As further preferred embodiment, first dispersant is preferably polyvinylpyrrolidone.Dispersant selection polyethylene after described One kind in alcohol, hydroxymethyl cellulose, sodium pyrophosphate, sodium pyrophosphate decahydrate, it is rear scattered as further preferred embodiment The preferred hydroxymethyl cellulose of agent or sodium pyrophosphate decahydrate.
Preferably, the initiator is redox initiation system, and reducing agent is preferably sodium hydrogensulfite, and oxidant is preferred For ammonium persulfate；The preferred sodium hydroxide of alkali formula compound.
Preferably, the nano inorganic powder is preferably nano silicon or nano titanium oxide, its particle diameter are 10- 50nm。
In the present invention, the amino acids metal ion chelate complex prepares gained by following process, will under the conditions of lucifuge Silver nitrate or zinc nitrate are dissolved in the Freamine Ⅲ of saturated concentration, or first by deionized water, amino acid in molar ratio (2.4-2.9):1 ratio mixing obtains Freamine Ⅲ, and then silver nitrate, zinc nitrate are dissolved in Freamine Ⅲ, its The mol ratio of middle silver nitrate or zinc nitrate and amino acid is (0.5-0.9):1,30-60min, mixing speed 600- is stirred at room temperature 800r/min, time 30-240min is reacted at room temperature, amino acid-Nano Silver chelate solution or amino acid-Nano-Zinc chelating is made Thing solution, it is stand-by, or amino acid-Nano Silver chelate powder or amino acid-Nano-Zinc is made further across filtering, drying Chelate powder, it is stand-by.The amino acid includes lysine, arginine, histidine, tryptophan, serine, threonine, sweet ammonia One or more combinations in acid, methionine.
In the present invention, the chitin metal salt ion chelate complex uses commercial goods, or according to prior art " one The preparation method (CN100435642C) of kind anti-tarnish chitosan complex silver antibacterial agent " is made.
In order to make further understanding to the present invention, it is explained in conjunction with embodiment, but these are described It is intended merely to further illustrate advantages and features of the invention, rather than limiting to the claimed invention.
Embodiment 1
Accurately weigh acrylic acid 200g, sodium hydroxide 70g, deionized water 210g, N, N '-methylene-bisacrylamide 0.2g, sodium hydrogensulfite 0.1g, ammonium persulfate 0.2g, polyvinylpyrrolidone 0.01g, hydroxymethyl cellulose 0.1g, poly- second two Alcohol diglycidyl ether, polyethylene glycol 200 press 1:Multiple crosslinking agent 0.6g, the nano silicon 10g of 1 mol ratio configuration, Antiseptic 2g.Wherein, the antiseptic of the present embodiment is chelating amino acids Nano Silver, and adds antiseptic in initial action cross-linking stage 1g, antiseptic 1g is added in the surface-crosslinked stage, using titanate coupling agent 0.2g, is then prepared according to the following steps：
1) sodium hydroxide is added after acrylic acid is mixed with deionized water to be neutralized.
2) polyvinylpyrrolidone, chelating amino acids Nano Silver are added into reaction system, is stirred rear sonic oscillation 12min, N, N '-methylene-bisacrylamide are added, continue to stir 5min, be then gradually heating to 35 DEG C, then add sulfurous Sour sodium, ammonium persulfate initiated polymerization 90s, obtain gelatinous polymer.
3) gelatinous polymer obtained by step (2) is granulated, is placed in drying 30min at a temperature of 158 DEG C, obtained Granulated polymer.
4) antiseptic pre-treatment step：Surplus antiseptic is configured to concentration with deionized water and is 30% solution, and is risen Temperature is to 30-45 DEG C, and addition nano silicon stirs in solution, and continues to disperse 10-20min using ultrasonic wave, will Chelating amino acids Nano Silver is fixed on the particle surface of nano silicon, filters after standing 30min, is resisted after vacuum drying Bacterium nano silicon.Then antimicrobial nano silica is placed in high-speed kneading machine, then adds titanate coupling agent and enter The coupling cladding processing of row high speed surface.
5) surface-crosslinked step：Multiple crosslinking agent is configured to concentration with deionized water and is 10% solution, and is heated up The antimicrobial nano silica of step (4) processing is added after to 30-45 DEG C, hydroxymethyl cellulose stirs, and continues to use Ultrasonic wave disperses 10-20min and obtains heat treatment crosslinked fluid, and this heat treatment crosslinked fluid is used into spray-on process pair at a temperature of 140 DEG C Gained granulated polymer carry out heat cross-linking surface treatment, be stirred mixing and heat drying after obtain there is three-dimensional cross-linked net The core-shell type bacteriostasis, and deodorization super absorbent resin of network structure.
Bacteriostasis, and deodorization super absorbent resin described in the present embodiment is inhaled so that the polyacrylate with certain degree of cross linking is high Water-base resin is matrix resin, and amino acid chela is combined between the molecular skeleton of the superabsorbent polyacrylate resin Nano Silver is closed, chelating amino acids Nano Silver is connected with the area load of super absorbent resin, for suppressing super absorbent resin Colloid breed bacteria and peculiar smell.
In the present embodiment, in bacteriostasis, and deodorization super absorbent resin, load is connected to the surface of super absorbent resin Antiseptic, as chelating amino acids Nano Silver is fixed on the particle surface of nano inorganic powder such as nano silicon, have long-acting Sustained-release antibacterial effect, meanwhile, antiseptic is because being carried on the carrier of nano inorganic powder, and therefore, antiseptic also will not be in height The problem of migration or transfer, occurs for the colloid surface formed after water-absorbing resins water swelling.Meanwhile it is carried on high-hydroscopicity tree The nano inorganic powder on fat surface, be advantageous to strengthen the gel strength of super absorbent resin colloid, increase super absorbent resin glue Such as the absorbability under 0.3psi, 0.7psi pressure under the logical fluidity and pressurized conditions of body, the absorption rate to liquid is improved, is fitted Close applied to the absorbing medium in ultrathin composite absorption core body in disposable absorbent article.
Embodiment 2
Acrylic acid 200g, sodium hydroxide 80g accurately are weighed, the degree of neutralization of the acrylic monomers solution of the present embodiment is 72%, deionized water 260g, N, N '-methylene-bisacrylamide 0.2g, sodium hydrogensulfite 0.1g, ammonium persulfate 0.2g, poly- second Alkene pyrrolidone 8g, sodium pyrophosphate decahydrate 6g, polyethyleneglycol diglycidylether, pentaerythrite press 1:The configuration of 1 mol ratio Multiple crosslinking agent 8g, nano titanium oxide 15g, antiseptic 20g.Wherein, the antiseptic of the present embodiment is by amino acid nano-silver chela Compound, chitosan nano silver ion chelate complex press mass fraction 1：1 ratio forms, and adds antiseptic in initial action cross-linking stage 10g, antiseptic 10g is added in the surface-crosslinked stage, using titanate coupling agent 0.2g, is then made by the step of embodiment 1 Core-shell type bacteriostasis, and deodorization super absorbent resin with three-dimensional crosslinked network structure.
Embodiment 3
In the present embodiment, antiseptic is not added in polymerization and the preliminary cross-linking stage of acrylic monomers, and antiseptic is added It is added on the surface treatment stage of multiple crosslinking agent.Acrylic acid 150g, sodium hydroxide 55g, deionized water 200g, N accurately are weighed, N '-methylene-bisacrylamide 0.1g, sodium sulfite 0.1g, sodium peroxydisulfate 0.2g, polyvinylpyrrolidone 3g, ten water pyrophosphoric acids Sodium 3g, polyethyleneglycol diglycidylether, pentaerythrite press 1:The multiple crosslinking agent 3g of 1 mol ratio configuration, nanometer titanium dioxide Titanium 15g, antiseptic 10g, using silane coupler 0.2g.Wherein, the antiseptic of the present embodiment by amino acid nano-silver chelate, Chitosan nano silver ion chelate complex presses mass fraction 1：Silver-series antibacterial agent 5g, the Tea Polyphenols 5g of 1 ratio composition, by the anti-of 10g Microbial inoculum was added in the surface-crosslinked stage, was then prepared according to the following steps：
1) sodium hydroxide is added after acrylic acid is mixed with deionized water to be neutralized.
2) polyvinylpyrrolidone is added into reaction system, is stirred rear sonic oscillation 12min, adds N, N '-Asia Bisacrylamide, continues to stir 5min, is then gradually heating to 35 DEG C, then adds sodium sulfite, ammonium persulfate triggers Polymerisation 90s, obtains gelatinous polymer.
3) gelatinous polymer obtained by step (2) is granulated, is placed in drying 30min at a temperature of 158 DEG C, obtained Granulated polymer.
4) the coupling processing step of nano inorganic powder：With deionized water by antiseptic be configured to concentration be 40% it is molten Liquid, and 30-45 DEG C is warming up to, nano titanium oxide is added in solution and is stirred, and 10-20min is disperseed using ultrasonic wave, Amino acid nano-silver chelate, chitosan nano silver ion chelate complex are fixed on to the particle surface of nano silicon, again Add Tea Polyphenols, continue ultrasonic wave disperse 10min after stand 30min after filter, vacuum drying after obtain antimicrobial nano titanium dioxide Titanium.Then antimicrobial nano titanium dioxide is placed in high-speed kneading machine, then adds silane coupler and carry out high speed surface coupling Cladding processing.
5) surface-crosslinked step：Multiple crosslinking agent is configured to concentration with deionized water and is 30% solution, and is heated up The antimicrobial nano titanium dioxide of step (4) processing is added after to 30-45 DEG C, sodium pyrophosphate decahydrate stirs, and continues to use Ultrasonic wave disperses 10-20min and obtains heat treatment crosslinked fluid, and this heat treatment crosslinked fluid is used into spray-on process pair at a temperature of 160 DEG C Gained granulated polymer carry out heat cross-linking surface treatment, be stirred mixing and heat drying after obtain there is three-dimensional cross-linked net The core-shell type bacteriostasis, and deodorization super absorbent resin of network structure.
Embodiment 4
In the present embodiment, antiseptic is not added in polymerization and the preliminary cross-linking stage of acrylic monomers, and antiseptic is straight In the solution for connecing the multiple crosslinking agent for making an addition to surface treatment stage.Accurately weigh acrylic acid 200g, sodium hydroxide 60g, go from Sub- water 220g, N, N '-methylene-bisacrylamide 0.1g, sodium sulfite 0.1g, sodium peroxydisulfate 0.2g, polyvinylpyrrolidone 0.01g, hydroxymethyl cellulose 3g, polyethyleneglycol diglycidylether, pentaerythrite press 1:The composite crosslinking of 1 mol ratio configuration Agent 2.5g, antiseptic 10g.Wherein, the antiseptic of the present embodiment is more by amino acid nano-silver chelate, carboxymethyl chitosan, tea Phenol presses 1:1:1 proportional arrangement forms, and is then prepared according to the following steps：
1) sodium hydroxide is added after acrylic acid is mixed with deionized water to be neutralized.
2) polyvinylpyrrolidone is added into reaction system, is stirred rear sonic oscillation 12min, adds N, N '-Asia Bisacrylamide, continues to stir 5min, is then gradually heating to 40 DEG C, then adds sodium sulfite, ammonium persulfate triggers Polymerisation 60s, obtains gelatinous polymer.
3) gelatinous polymer obtained by step (2) is granulated, is placed in drying 30min at a temperature of 158 DEG C, obtained Granulated polymer.
4) multiple crosslinking agent is configured to concentration with deionized water and is 30% solution, and be warming up to 30-45 DEG C, in solution Dispersant stirs after interior addition, then proceedes to add antiseptic, and continues to disperse 10-20min acquisition heat using ultrasonic wave Handle crosslinked fluid；Finally, this heat treatment crosslinked fluid is gathered at a temperature of 160 DEG C using spray-on process to graininess obtained by step (3) Compound carries out heat cross-linking surface treatment, and the shell core with three-dimensional crosslinked network structure is obtained after being stirred mixing and heat drying Type bacteriostasis, and deodorization super absorbent resin.
Embodiment 5
The present embodiment is using commercially available common super absorbent resin as control sample, respectively to made from embodiment 1 to embodiment 4 Super absorbent resin carries out absorbent properties, Anti-microbial Performance Tests.Experimental condition is as follows：
1) absorbent properties of super absorbent resin are tested according to condition as defined in GB/T22905-2008.
2) the Anti-microbial Performance Tests method of super absorbent resin：First, the high suction of 0.2g embodiments 1,2,3,4 is weighed respectively Water-base resin, it is put into after sterilized processing in 200ml sterilizing conical flask, adds the physiology salt of the sterilized processing of 60ml Water, it is set to fully absorb swelling.Secondly, the strains such as Escherichia coli, staphylococcus aureus, candida albicans are accessed into fluid nutrient medium In, 24h is swayed in 37 DEG C, 180ppm shaking table and forms bacterium solution.Finally, take 1ml activate after bacterium solution add conical flask in 37 DEG C, sway 8h in 180ppm shaking table, after bacterium solution is pipetted from conical flask and is diluted, the growth of bacterium is observed by applying flat board Situation, and calculate bacteriostasis rate.
Result of the test is as shown in the table：
The present embodiment result shows exist instant invention overcomes nano-silver ionic as antiseptic and be not sufficiently stable, and easily turns Become argent or silver oxide and produce discoloration, the problem of seriously reducing its antibacterial ability.The amino acid metal salt of the present invention Coordination ion in ion chelate complex, chitin metal salt ion chelate complex has good slow releasing function, so that metal Ion has efficient, the lasting, effect of broad-spectrum antiseptic.
Embodiment 6
The present embodiment provides a kind of absorbent article using bacteriostasis, and deodorization super absorbent resin, comprising liquid permeability surface layer, no Liquid permeability bottom and the absorptive core between liquid permeability surface layer and opaque liquid bottom, its feature are in the absorption Embodiment 1, embodiment 2, embodiment 3 or bacteriostasis, and deodorization super absorbent resin made from embodiment 4 are combined with core body.
The present embodiment absorptive core is composite absorption core body, and the composite absorption core body includes loft nonwoven layer of cloth, should Loft nonwoven layer of cloth is to crimp hot-melt fiber with height, or with height curling hot-melt fiber, scroll pile pulp fibres by wearing The built-up fluffy fiber network of winding is inserted, upper epidermis, layer in loft nonwoven layer of cloth lay bacteriostasis, and deodorization respectively Super absorbent resin, absorbed layer, lower absorbed layer in formation, the bacteriostasis, and deodorization high-hydroscopicity tree in upper absorbed layer, lower absorbed layer Fat be implanted into respectively the upper epidermis of fluffy fiber network, layer fiber mesh in, by upper absorbed layer, lower absorbed layer with it is fluffy non- Woven layer is connected as a single entity, at the same upper absorbed layer, lower absorbed layer extexine on glued connection top layer coating, bottom respectively Coating.
In the absorbent article described in the present embodiment, in addition to the closed group for being maintained at body assembly with wearer Part, closed component include the open type closed-system being made up of left and right waist patch with frontal waist plaster or by elastomeric material ring waist closure and The pants type closed-system of structure.
By the absorbent article 100 of the present embodiment, its feature is that embodiment 1 is combined with the absorptive core to be made The bacteriostasis, and deodorization super absorbent resin obtained.20 consumers are distributed to by every consumer 5 to try out, while every consumer is another The commercially available regular absorbent product sample as a comparison of hair 3, the age bracket of infant for the one full year of life of age bracket 2-year one full year of life half, wherein, Boy baby's accounting 55%, girl baby's accounting 45%, it is desirable to which the father and mother of every trier fill in per a piece of absorbent article strictly according to the facts after on probation Status investigation list on probation.
At present, had problems in that in disposable absorbent article industry, after super absorbent resin absorbs human urine, by The urea in human urine can be decomposed in bacterium and ammonia stink occurs, and the present embodiment is by suppressing the growth of bacterium, therefore from source The generation of ammonia stink is inhibited on head.And ammonia stink carries out intuitive judgment by the smell of people.Wherein：
1) use habit investigation is summarized as follows：
2) absorbability and bacteriostasis, and deodorization situation are summarized as follows shown in table.
Show from the result on trial of absorbent article, bacteriostasis, and deodorization super absorbent resin of the invention to the excreta of human body, As urine not only has excellent absorbent properties, while there is preferable inhibition to bacterium, can effectively suppress to absorb system Product grow Escherichia coli, staphylococcus aureus, candida albicans in use, the tender skin of care infant, effectively keep away Exempt from erythema and the Peculiar Smell that existing absorbent article often occurs in use.
Although the present invention describes specific case study on implementation, the scope of the present invention is not limited to above-mentioned specific real Example is applied, without departing from the case in the spirit of the invention, various modifications, variations and alternatives to the present invention each fall within the guarantor of the present invention Protect scope.

Claims (10)

  1. A kind of 1. bacteriostasis, and deodorization super absorbent resin, it is characterised in that：
    1) the bacteriostasis, and deodorization super absorbent resin be using the superabsorbent polyacrylate resin with certain degree of cross linking as Matrix resin, antimicrobial composition is combined between the network molecule chain in the super absorbent resin, or/and in high water absorption Property resin surface three-dimensional crosslinked network structure in be loaded with antimicrobial composition, for suppress super absorbent resin colloid grow Bacterium and peculiar smell, the antimicrobial composition are in amino acid metal salt ion chelate complex, chitin metal salt ion chelate complex One or two kinds of compositions；
    2) super absorbent resin be through deionized water dilute and by alkali formula compound in and acrylic monomers solution form Acrylic acid/acrylates mixed liquor in, add just crosslinking agent, first dispersant and the antibacterial for being stirring evenly and then adding into 0-80% Agent composition continues to stir, and is warming up to 35 DEG C -70 DEG C and adds the colloidal super absorbent resin that initiator is polymerized, right The colloidal super absorbent resin passes sequentially through granulation, dried, and is used at a temperature of 110-180 DEG C mainly by multiple crosslinking agent The composite antibacterial crosslinking agent formed with 20%-100% resistance agent composition and the rear dispersant configuration of 0.05-3 parts is carried out Polyacrylate core-shell type super absorbent resin of the acquisition with three-dimensional crosslinked network structure for being surface-treated and being formed；
    3) count in parts by weight, the antimicrobial composition of monomer 0.05-50 parts in 100 parts of acrylic acid.
  2. 2. bacteriostasis, and deodorization super absorbent resin according to claim 1, it is characterised in that：The composite antibacterial crosslinking agent by 20%-100% antiseptic and described multiple crosslinking agent, rear dispersant, deionized water are configured and formed, composite antibacterial crosslinking The concentration of agent be 5%-50% solution, 30-45 DEG C of solution temperature.
  3. 3. bacteriostasis, and deodorization super absorbent resin according to claim 1, it is characterised in that：The antimicrobial composition composition Formula also includes nano inorganic powder and coupling agent, counts in parts by weight, nano inorganic powder is 0.1-30 parts；The coupling The addition of agent is the 0.5%-3.5% of nano inorganic powder parts by weight；
    It is the molten of 30%-70% that 20%-100% antiseptic is configured to concentration by the composite antibacterial crosslinking agent with deionized water Liquid, adds nano inorganic powder after being warming up to 30-50 DEG C, stirring and ultrasonic wave disperse 10-20min, antiseptic is uniformly fixed Filtered after the particle surface of nano inorganic powder, standing 30-60min, obtain antimicrobial nano inorganic particle after vacuum drying, and Surface coupling processing is carried out to antibacterial nano inorganic powder and obtains antimicrobial nano inorganic particle, then with deionized water by compound friendship Connection agent is configured to the solution that concentration is 5%-50%, and is warming up to 30-45 DEG C, then by the antimicrobial nano inorganic particle, rear scattered Agent is added and stirred, and is continued ultrasonic wave 10-20min and divided equally the scattered heat treatment crosslinked fluid formed.
  4. 4. bacteriostasis, and deodorization super absorbent resin according to claim 1, it is characterised in that：The amino acids metal ion chela Compound includes amino acid nano-silver ion chelate complex, amino acid Nano-Zinc ion chelate complex；The chitosan-metal salt ion chela Compound includes chitosan nano silver ion chelate complex, chitosan nano Zinc Ions Chelated thing.
  5. 5. bacteriostasis, and deodorization super absorbent resin according to claim 1, it is characterised in that：Dispersant selects poly- second after described One kind in enol, hydroxymethyl cellulose, sodium pyrophosphate, sodium pyrophosphate decahydrate.
  6. 6. bacteriostasis, and deodorization super absorbent resin according to claim 1, it is characterised in that：Count in parts by weight, the height The composition and parts by weight of water-absorbing resins are as follows：
    100 parts of acrylic acid；
    Alkali formula compound 35-45 parts；
    Deionized water 105-145 parts；
    First crosslinking agent 0.006-1.8 parts；
    Initiator 0.005-2 parts；
    First dispersant 0.005-4 parts；
    Multiple crosslinking agent 0.3-4 parts；
    The just crosslinking agent is N, N '-methylene-bisacrylamide, polyethylene glycol 200, butanediol, pentaerythrite, trihydroxy methyl One kind in methane triacrylate；The multiple crosslinking agent is ethers, esters, is crosslinked containing two and two or more hydroxy alcohols Wherein at least a kind of composition in agent；
    One kind in the just dispersant selection polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone；The initiator is oxidation Reduction initiating system, reducing agent are bisulfites, the anti-different bad one of which learned in hydrochlorate；Oxidant is selected from persulfuric acid One of which in salt, hydrogen peroxide；Alkali formula compound chooses the one of which in sodium hydroxide, potassium hydroxide.
  7. 7. bacteriostasis, and deodorization super absorbent resin according to claim 6, it is characterised in that：The ethers crosslinking agent is using poly- Ethylene glycol diglycidylether, the esters crosslinking agent is using polyethylene glycol 200 diacrylate, the propylene of Pehanorm three One or both of acid esters, the crosslinkers are wherein at least one in polyethylene glycol 200, butanediol, pentaerythrite Kind is formed.
  8. 8. bacteriostasis, and deodorization super absorbent resin according to claim 3, it is characterised in that：The nano inorganic powder is to receive One or both of rice silica, nano titanium oxide, nano aluminium oxide combination, the particle diameter of the nano inorganic powder are 10-50nm；The coupling agent is aluminate coupling agent, titanate coupling agent or silane coupler.
  9. 9. a kind of absorbent article of bacteriostasis, and deodorization super absorbent resin using as described in any right of claim 1 to 8, comprising Liquid permeability surface layer, opaque liquid bottom and the absorptive core between liquid permeability surface layer and opaque liquid bottom, its feature It is：Bacteriostasis, and deodorization super absorbent resin in the absorptive core with reference to described in just like any right of claim 1 to 8.
  10. 10. the absorbent article according to claim 9 using bacteriostasis, and deodorization super absorbent resin, it is characterised in that：It is described Absorptive core is composite absorption core body, and the composite absorption core body includes loft nonwoven layer of cloth, and the loft nonwoven layer of cloth is Hot-melt fiber is crimped with height, or it is built-up by interspersed winding with height curling hot-melt fiber, scroll pile pulp fibres Fluffy fiber network, upper epidermis, layer in loft nonwoven layer of cloth lay bacteriostasis, and deodorization super absorbent resin respectively, are formed Upper absorbed layer, lower absorbed layer, the bacteriostasis, and deodorization super absorbent resin in upper absorbed layer, lower absorbed layer are implanted into fluffy fiber respectively In the upper epidermis of network, the fiber mesh of layer, upper absorbed layer, lower absorbed layer and loft nonwoven layer of cloth are connected as a single entity, Simultaneously upper absorbed layer, lower absorbed layer extexine on glued connection top layer coating, bottom coating respectively.
CN201710671956.8A 2017-08-08 2017-08-08 A kind of bacteriostasis, and deodorization super absorbent resin and the absorbent article containing the super absorbent resin Pending CN107501462A (en)

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Application publication date: 20171222