CN108102268A - A kind of tea polyphenols/high hydroscopic resin particle and its preparation method and application - Google Patents
A kind of tea polyphenols/high hydroscopic resin particle and its preparation method and application Download PDFInfo
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- CN108102268A CN108102268A CN201711472421.4A CN201711472421A CN108102268A CN 108102268 A CN108102268 A CN 108102268A CN 201711472421 A CN201711472421 A CN 201711472421A CN 108102268 A CN108102268 A CN 108102268A
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- 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
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- 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
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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
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- 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
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K3/36—Silica
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/216—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with other specific functional groups, e.g. aldehydes, ketones, phenols, quaternary phosphonium groups
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- 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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- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
- C08K2003/3081—Aluminum sulfate
Abstract
The present invention relates to a kind of tea polyphenols/high hydroscopic resin particles and its preparation method and application.Preparation method：(1) 200~300 parts by weight of acrylic acid are dissolved, is configured to the acrylic acid solution that concentration is 20~60wt%, is adjusted the pH of solution to 6~7 with alkaline matter；(2) 2~6 parts by weight of crosslinking agent are added in into acrylic acid solution, add in 0.5~2 parts by weight initiator after mixing, under the initiation of initiator polymerisation occurs for mixed solution；After polymerisation, obtained colloid is made to the resin particle of 30~80 mesh；(3) 100 parts by weight resin particles and 1~3 parts by weight inert inorganic salt powder are uniformly mixed, add 0.5~1.5 parts by weight tea polyphenols and the surface-crosslinked liquid of 20~25 parts by weight, it is uniformly mixed, mixture is subjected to isothermal holding at 150~190 DEG C, being made has excellent antibacterial performance, and the high hydroscopic resin particle of adsorbable peculiar smell.
Description
Technical field
The present invention relates to high-molecular compound technical field more particularly to a kind of tea polyphenols/high hydroscopic resin particle and its
Preparation method and application.
Background technology
High hydroscopic resin (be otherwise known as SAP) is widely used in paper diaper when with superpower suction water holding capacity, defends
The hygiene article sectors such as raw towel.Paper diaper, sanitary napkin etc. are obtained by the technological innovation of decades in comfort and dry-ness aspect
Tremendous development has been arrived, the variation of matter is had occurred that compared with performances such as early production paper diaper of today, sanitary napkins, but still
So there are antibiotic property it is poor, have the problems such as peculiar smell, this is also the problem of long-standing problem sanitary goods industry.
Tea polyphenols are all natural antioxidant extracted from tealeaves, are the general names of Polyphenols of Tea, including
Flavanol compound, anthocyanin class, flavonoids, flavonols and phenolic acid class etc., wherein most being attached most importance to flavanol compound substance (catechin)
It will.Whole world research tea polyphenols have more than hundred years history, long-term research, analysis, practical application, at present it is known that tea polyphenols have
Following functions：Eliminate harmful free radicals, very strong antioxidation, anti-aging effects, radiation resistance, antitumor to cancer cell
Inhibitory action, antibiotic and sterilizing, antivirus action, antiatherosclerosis, enhancing cardiac function, anti-arrhythmia, prevention brain
Ischemical reperfusion injury, anti-moth shield tooth, skin whitening, reduction wrinkle etc..Above-mentioned function based on tea polyphenols, it is widely used
In fields such as food, medicine, daily use chemicals.
Application publication number is to disclose a kind of utilization tea polyphenols in the application documents of CN103588924A to prepare super absorbent resin
The method of fat adds in tea polyphenols in polymerization stage, and tea polyphenols is made to participate in polymerisation, and final tea polyphenols-height obtained is inhaled
Water-resin joint product.Although the joint product has preferable bacteriostasis property, which is in polymerisation rank
Section adds in tea polyphenols, so that tea polyphenols are wrapped in the inside of the high hydroscopic resin with three-dimensional net structure, causes height
The bacteriostasis property of water-absorbing resin is subject to a degree of influence.Moreover, because the package of three-dimensional net structure, tea polyphenols are had
The function of absorption peculiar smell also receive very big limitation, cause joint product that can not play the role of deodorization and eliminate the unusual smell, limit
It is in the application of the hygiene article sectors such as paper diaper, sanitary napkin.
(1) technical problems to be solved
For above-mentioned technical problem, the present invention provides a kind of tea with excellent antibacterial performance and absorption peculiar smell performance is more
The preparation method of phenol/high hydroscopic resin particle.
(2) technical solution
In order to solve the above technical problem, the present invention provides following technical solutions：
A kind of preparation method of tea polyphenols/high hydroscopic resin particle, the preparation method include the following steps：
(1) 200~300 parts by weight of acrylic acid are dissolved, is configured to the acrylic acid solution that concentration is 25~60wt%, then
The pH of acrylic acid solution is adjusted to 6~7 with alkaline matter；
(2) 2~6 parts by weight of crosslinking agent are added in into acrylic acid solution, 0.5~2 parts by weight is added in after mixing and triggers
Under the initiation of initiator polymerisation occurs for agent, mixed solution；After polymerisation, obtained colloid is made 30~80
Purpose resin particle；
(3) 100 parts by weight resin particles and 1~3 parts by weight inert inorganic salt powder are uniformly mixed, add 0.5~
1.5 parts by weight tea polyphenols and the surface-crosslinked liquid of 20~25 parts by weight, be uniformly mixed, then by mixture at 150~190 DEG C into
Row isothermal holding, so as to obtain tea polyphenols/high hydroscopic resin particle.
Preferably, in step (3), the inert inorganic salt powder is selected from calcium oxide, kaolin, silica, sulfuric acid
Any one of aluminium, aluminium oxide, calcium carbonate and magnesium carbonate are a variety of.
Preferably, in step (3), the surface-crosslinked liquid is selected from multicomponent alcoholics compound, polyhydric amine compounds, epoxy
Any one of compound is a variety of；
Preferably, the multicomponent alcoholics compound is selected from any one of ethylene glycol, butanediol, glycerine, triethylene glycol
It is or a variety of；The polynary aminated compounds is selected from any one of ethylenediamine, diethylene triamine, triethylenediamine or a variety of；And/or institute
Epoxide is stated in butanediol diglycidyl ether, polyglycerol polyglycidyl ether, sorbierite polyglycidyl ether
It is any one or more.
Preferably, in step (3), tea polyphenols used are food-grade, and purity is more than 99%.
Preferably, in step (2), the crosslinking agent is selected from N, N- methylene diacrylamines, N- methylol acryloyls
Any one of amine, tetraallyloxyethane, trimethylolpropane tris propylene acid esters are a variety of；And/or
The initiator is redox initiator, includes Oxidizing and Reducing Agents；The oxidant is selected from benzoyl peroxide
Any one of formyl, isopropyl benzene hydroperoxide, potassium peroxydisulfate, the reducing agent are selected from two hydration sodium bisulphite formaldehydes, sulphur
Any one of sour ferrous, sodium hydrogensulfite；Preferably, the reductant-oxidant is potassium peroxydisulfate and sodium hydrogensulfite.
Preferably, in step (2), the polymerisation is triggered at 5~15 DEG C；Preferably, trigger at 8~10 DEG C
The polymerisation.
Preferably, in step (2), the resin particle is prepared as follows：
Micelle is made by being granulated in colloid, then dries micelle obtained at 120~150 DEG C, then will be after drying
Micelle be ground into particle, particle is sieved, so as to be made 30~80 mesh resin particle.
A kind of tea polyphenols/high hydroscopic resin particle, are made using above-mentioned preparation method.Preferably, the tea polyphenols/height is inhaled
The antibiotic rate of water-resin particle is more than 97%.
Above-mentioned tea polyphenols/application of the high hydroscopic resin particle in hygienic articles；Preferably, the hygienic articles are urinated for paper
Any one of trousers, sanitary napkin, panty liner.
(3) advantageous effect
The above-mentioned technical proposal of the present invention has the following advantages that：
This is in using the indices of tea polyphenols made from preparation method provided by the invention/high hydroscopic resin particle
Industry-leading is horizontal, has excellent water imbibition, water-retaining property, infiltration rate and logical liquid speed degree, can meet baby paper diaper, into
The requirement of the hygienic articles such as people's paper diaper, female sanitary towel or feminine hygiene pads.What is more important is provided using the present invention
Preparation method made from tea polyphenols/high hydroscopic resin particle also have the function of excellent anti-microbial property and absorption peculiar smell, make
Its comprehensive performance is more excellent, and adding in the high hydroscopic resins of tea polyphenols, not only bacteriostasis greatly enhances, such as to staphylococcus, big
The inhibitory action such as enterobacteria, hay bacillus are apparent, can also adsorb peculiar smell with certain deodorization, be obtained with the method
Tea polyphenols/high hydroscopic resin particle is more suitable for applying in the hygiene article sectors such as high-end paper diaper and sanitary napkin.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is the part of the embodiment of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
On the premise of all other embodiments obtained, belong to the scope of protection of the invention.
The present invention provides a kind of preparation method of tea polyphenols/high hydroscopic resin particle, preparation method includes the following steps：
(1) 200~300 parts by weight of acrylic acid are dissolved, is configured to the acrylic acid solution that concentration is 25~60wt%, then
The pH of acrylic acid solution is adjusted to 6~7 with alkaline matter.In this step, alkaline matter used be selected from sodium hydroxide or
Potassium hydroxide.When preparing acrylic acid solution, solvent used can be deionized water, can be ultra-pure water, can also be distillation
Water.
(2) 2~6 parts by weight of crosslinking agent are added in into acrylic acid solution, 0.5~2 parts by weight is added in after mixing and triggers
Under the initiation of initiator polymerisation occurs for agent, mixed solution；After polymerisation, colloid obtained by the reaction is made 30
The resin particle of~80 mesh.Crosslinking agent preferably is selected from N, N- methylene diacrylamines, N hydroxymethyl acrylamide, four allyloxys
Any one of ethane, trimethylolpropane tris propylene acid esters are a variety of.Initiator is redox initiator, includes oxidant
And reducing agent；The oxidant is selected from any one of benzoyl peroxide, isopropyl benzene hydroperoxide, potassium peroxydisulfate, described to go back
Former agent is selected from any one of two hydration sodium bisulphite formaldehydes, ferrous sulfate, sodium hydrogensulfite；Preferably, the oxidation is gone back
Former agent is potassium peroxydisulfate and sodium hydrogensulfite.In some embodiments, initiator initiated polymerization at 5~15 DEG C, it is more excellent
Elect the initiated polymerization at 8~10 DEG C as.The resin particle is prepared as follows：Colloid is made by being granulated
Into micelle, then micelle obtained at 120~150 DEG C is dried, then the micelle after drying is ground into particle, by particle into
Row screening, so as to which the resin particle of 30~80 mesh be made.
(3) 100 parts by weight resin particles and 1~3 parts by weight inert inorganic salt powder are uniformly mixed, add 0.5~
1.5 parts by weight tea polyphenols and the surface-crosslinked liquid of 20~25 parts by weight, be uniformly mixed, then by mixture at 150~190 DEG C into
Row isothermal holding, so as to obtain tea polyphenols/high hydroscopic resin particle.Inert inorganic salt powder preferably is selected from calcium oxide, kaolin, two
Any one of silica, aluminum sulfate, aluminium oxide, calcium carbonate and magnesium carbonate are a variety of.Surface-crosslinked liquid preferably is selected from polyalcohols
Any one of compound, polyhydric amine compounds, epoxide are a variety of；Preferably, the multicomponent alcoholics compound is selected from
Any one of ethylene glycol, butanediol, glycerine, triethylene glycol are a variety of；The polynary aminated compounds is selected from ethylenediamine, two
Any one of ethylenediamine, triethylenediamine are a variety of；And/or the epoxide is selected from butanediol diglycidyl ether, gathers
Any one of glycerine polyglycidyl ether, sorbierite polyglycidyl ether are a variety of.Tea polyphenols used are food-grade, pure
Degree is more than 99%.Intensity difference without surface-crosslinked high hydroscopic resin particle, pressurizing absorption amount is low, is not suitable for paper urine
The larger hygienic articles of the liquid absorption amounts such as trousers, sanitary napkin, panty liner.Add in surface-crosslinked liquid can improve resin uptake and
Infiltration rate, but due to the addition of tea polyphenols, add surface-crosslinked difficulty, resin particle surfaces can be caused to occur largely not
The part crosslinked.In order to overcome the above problem, the present invention adds suitable inert inorganic salt powder in preparation method
And to the optimization of surface-crosslinked process conditions.The addition of inert inorganic salt powder can extend surface-crosslinked liquid and particle surface into
The time of row reaction, uniformly resin particle surfaces are coated so as to be more advantageous to surface-crosslinked liquid.
The present invention also provides a kind of tea polyphenols/high hydroscopic resin particles, are made using above-mentioned preparation method.Tea obtained
The antibiotic rate of polyphenol/high hydroscopic resin particle is more than 97%.
Above-mentioned tea polyphenols/high hydroscopic resin particle can be applied to the hygienic articles such as paper diaper, sanitary napkin, panty liner
In.
It is the embodiment that the present invention enumerates below.
Embodiment 1
It prepares raw material and includes following component：200 parts by weight of acrylic acid, 2.6 parts by weight of tetraallyloxyethane, potassium peroxydisulfate
0.8 parts by weight, 0.5 parts by weight of sodium hydrogensulfite, 1 parts by weight of aluminum sulfate, 0.5 parts by weight of silica, 15 parts by weight of ethylene glycol,
7.4 parts by weight of butanediol diglycidyl ether, 0.6 parts by weight of tea polyphenols.
Preparation method includes the following steps：
Acrylic acid is dissolved in deionized water, is configured to the acrylic acid solution that concentration is 22wt%, it will with sodium hydroxide
The pH value of acrylic acid solution is adjusted to 6~7, adds tetraallyloxyethane, and is uniformly mixed, then add in potassium peroxydisulfate and
Sodium hydrogensulfite triggers mixed solution that polymerisation occurs at 10 DEG C.
After polymerisation, gluey reaction product is granulated, micelle is made.Then micelle at 120 DEG C is dried, dried
It is crushed again after dry, particle is made.By particle screening, the resin particle of 30 mesh is made.
Aluminum sulfate is added in into 100 parts by weight resin particles and silica is uniformly mixed, then tea polyphenols and surface are handed over
The connection mixed mixed liquor of liquid is added in resin particle, and is stirred evenly, and then keeps the temperature 20 minutes at 180 DEG C, heat preservation knot
Beam postcooling is to room temperature, so as to which tea polyphenols/high hydroscopic resin particle be made.
Tea polyphenols obtained/high hydroscopic resin particle has following property：
Inhale distilled water multiple：500 times；
Inhale 0.9% physiological saline：66 times；
Water retention：35 times；
Pressurizing absorption (0.3Psi)：35 times；
Pressurizing absorption (0.7Psi)：25 times；
Pressurizing absorption (0.9Psi)：18 times；
Infiltration rate：25s；
Logical liquid speed degree：200mL/min.
Embodiment 2
It prepares raw material and includes following component：230 parts by weight of acrylic acid, 3.5 parts by weight of trimethylolpropane trimethacrylate,
1.1 parts by weight of potassium peroxydisulfate, 2.4 parts by weight of sodium hydrogensulfite, 1.5 parts by weight of aluminium oxide, 1 parts by weight of kaolin, glycerine 15
Parts by weight, 8.5 parts by weight of polyglycerol polyglycidyl ether, 0.8 parts by weight of tea polyphenols.
Preparation method includes the following steps：
Acrylic acid is dissolved in deionized water, is configured to the acrylic acid solution that concentration is 25wt%, it will with sodium hydroxide
The pH value of acrylic acid solution is adjusted to 6~7, adds trimethylolpropane trimethacrylate, and is uniformly mixed, and then adds in
Potassium sulfate and sodium hydrogensulfite trigger mixed solution that polymerisation occurs at 15 DEG C.
After polymerisation, gluey reaction product is granulated, micelle is made.Then micelle at 150 DEG C is dried, dried
It is crushed again after dry, particle is made.By particle screening, the resin particle of 80 mesh is made.
Aluminium oxide is added in into resin particle and kaolin is uniformly mixed, then tea polyphenols and surface-crosslinked liquid are mixed
Mixed liquor is added in resin particle, and is stirred evenly, and then keeps the temperature 20 minutes at 190 DEG C, room is cooled to after heat preservation
Temperature, so as to which hydroscopic high-molecular resin particle be made.
Hydroscopic high-molecular resin obtained has following property：
Inhale distilled water multiple：470 times；
Inhale 0.9% physiological saline：65 times；
Water retention：34.5 times；
Pressurizing absorption (0.3Psi)：34 times；
Pressurizing absorption (0.7Psi)：23 times；
Pressurizing absorption (0.9Psi)：17 times；
Infiltration rate：26s；
Logical liquid speed degree：180mL/min.
Embodiment 3
It prepares raw material and includes following component：275 parts by weight of acrylic acid, 1.8 parts by weight of trimethylolpropane trimethacrylate,
0.75 parts by weight of N, N- methylene diacrylamine, 0.9 parts by weight of potassium peroxydisulfate, 0.4 parts by weight of sodium hydrogensulfite, calcium carbonate
0.5 parts by weight, silica 1 .0 parts by weight, 10 parts by weight of triethylene glycol, 10 parts by weight of ethylenediamine, 1.0 parts by weight of tea polyphenols.
Preparation method includes the following steps：
Acrylic acid is dissolved in deionized water, is configured to the acrylic acid solution that concentration is 25wt%, it will with sodium hydroxide
The pH value of acrylic acid solution is adjusted to 6~7, adds trimethylolpropane trimethacrylate and N, two acryloyl of N- methylene
Amine, and be uniformly mixed, it then adds in potassium peroxydisulfate and sodium hydrogensulfite triggers mixed solution that polymerisation occurs at 15 DEG C.
After polymerisation, gluey reaction product is granulated, micelle is made.Then micelle at 150 DEG C is dried, dried
It is crushed again after dry, particle is made.By particle screening, the resin particle of 50 mesh is made.
Calcium carbonate is added in into resin particle and silica is uniformly mixed, then will be after tea polyphenols and the mixing of surface-crosslinked liquid
Mixed liquor be added in resin particle, and stir evenly, then keep the temperature 20 minutes at 160 DEG C, be cooled to after heat preservation
Room temperature, so as to which tea polyphenols/high hydroscopic resin particle be made.
Hydroscopic high-molecular resin obtained has following property：
Inhale distilled water multiple：480 times；
Inhale 0.9% physiological saline：67 times；
Water retention：39 times；
Pressurizing absorption (0.3Psi)：28 times；
Pressurizing absorption (0.7Psi)：21 times；
Pressurizing absorption (0.9Psi)：16 times；
Infiltration rate：22s；
Logical liquid speed degree：140mL/min.
Embodiment 4
It prepares raw material and includes following component：300 parts by weight of acrylic acid, 1.8 parts by weight of tetraallyloxyethane, N- methylols
3.5 parts by weight of acrylamide, 1.2 parts by weight of potassium peroxydisulfate, 0.7 parts by weight of sodium hydrogensulfite, 2 parts by weight of magnesium carbonate, titanium dioxide
1 parts by weight of silicon, 16 parts by weight of butanediol, 5.5 parts by weight of sorbierite glycidol ether, 1.5 parts by weight of tea polyphenols.
Preparation method includes the following steps：
Acrylic acid is dissolved in deionized water, is configured to the acrylic acid solution that concentration is 34wt%, it will with sodium hydroxide
The pH value of acrylic acid solution is adjusted to 6~7, adds tetraallyloxyethane and N hydroxymethyl acrylamide, and is uniformly mixed,
Then add in potassium peroxydisulfate and sodium hydrogensulfite triggers mixed solution that polymerisation occurs at 15 DEG C.
After polymerisation, gluey reaction product is granulated, micelle is made.Then micelle at 150 DEG C is dried, dried
It is crushed again after dry, particle is made.By particle screening, the resin particle of 50 mesh is made.
Magnesium carbonate is added in into resin particle and silica is uniformly mixed, then will be after tea polyphenols and the mixing of surface-crosslinked liquid
Mixed liquor be added in resin particle, and stir evenly, then keep the temperature 20 minutes at 170 DEG C, be cooled to after heat preservation
Room temperature, so as to which tea polyphenols/high hydroscopic resin particle be made.
Hydroscopic high-molecular resin obtained has following property：
Inhale distilled water multiple：450 times；
Inhale 0.9% physiological saline：63 times；
Water retention：35 times；
Pressurizing absorption (0.3Psi)：36 times；
Pressurizing absorption (0.7Psi)：24 times；
Pressurizing absorption (0.9Psi)：18 times；
Infiltration rate：27s；
Logical liquid speed degree：190mL/min.
Comparative example 1
Tea polyphenols are not included in the preparation component of comparative example 1, remaining component is identical with embodiment 4.
Preparation method is identical with embodiment 4, comparison sample 1 is made, performance is as follows：
Inhale distilled water multiple：445 times；
Inhale 0.9% physiological saline：63 times；
Water retention：35 times；
Pressurizing absorption (0.3Psi)：35 times；
Pressurizing absorption (0.7Psi)：23.5 times；
Pressurizing absorption (0.9Psi)：18 times；
Infiltration rate：28s；
Logical liquid speed degree：180mL/min.
Comparative example 2
Tea polyphenols are not included in the preparation component of comparative example 2, remaining component is identical with embodiment 1.Preparation method is the same as implementation
Example 1 is identical, comparison sample 2 is made, performance is as follows：
Inhale distilled water multiple：503 times
Inhale 0.9% physiological saline：65.5 times；
Water retention：35 times；
Pressurizing absorption (0.3Psi)：34.5 times；
Pressurizing absorption (0.7Psi)：25.5 times；
Pressurizing absorption (0.9Psi)：18 times；
Infiltration rate：24s；
Logical liquid speed degree：200mL/min.
Comparative example 3
The preparation component of comparative example 3 is essentially identical with embodiment 1, the difference is that：The surface-crosslinked liquid includes second
10 parts by weight of 20 parts by weight of glycol and butanediol diglycidyl ether；Preparation method is essentially identical with embodiment 1, and difference exists
In：Holding temperature is 120 DEG C, and soaking time is 50 minutes.Comparison sample 3 obtained has following index：
Inhale distilled water multiple：437 times；
Inhale 0.9% physiological saline：55 times；
Water retention：31 times；
Pressurizing absorption (0.3Psi)：29 times；
Pressurizing absorption (0.7Psi)：19 times；
Pressurizing absorption (0.9Psi)：12 times；
Infiltration rate：31s；
Logical liquid speed degree：85mL/min.
Comparative example 4
It is prepared by the preparation method in application documents for being CN103588924A according to application publication number：Accurately weigh
25.00g NaOH measure 100mL distilled water, 25% NaOH solution are configured to, under ice-water bath and stirring condition, with 50g third
Olefin(e) acid carries out neutralization reaction.0.01g N, N '-methylene-bisacrylamide are weighed, 20mL distilled water is dissolved in and is made into aqueous solution, to
The aqueous solution of 20mL N, N '-methylene-bisacrylamide, stirring are added in the acrylic acid and its sodium-salt aqueous solution that have neutralized
5min, then add 0.07g K2S2O8Initiator is stirred to it and is completely dissolved.Again into the reaction system add in 10mL dissolved with
The aqueous solution of 0.035g tea polyphenols stirs simultaneously mixing.The mixed solution obtained is placed in baking oven, in 80 DEG C of polymerisation 2h,
By gained clear gel cooling, shearing, dry to get granular high hydroscopic resin, as a comparison sample 4.
Inhale distilled water multiple：950 times；
Inhale 0.9% physiological saline：70 times；
Water retention：33 times；
Pressurizing absorption (0.3Psi)：35 times；
Pressurizing absorption (0.7Psi)：26 times；
Pressurizing absorption (0.9Psi)：18 times；
Infiltration rate：25s；
Logical liquid speed degree：200mL/min.
Anti-microbial property detects
Testing principle：It is shaken for a long time by quick in a liquid, increases contact of the experimental bacteria with antimicrobial sample to show
Its bacteriostasis compared with control sample, calculates the percentage of bacterium reduction on antimicrobial sample and sentences so as to be made to its antibacterial ability
It is disconnected.
Detecting step：(1) prepared by bacterium solution：The fresh broth culture of Escherichia coli for 24 hours is taken, 20min is stood after shaking up, it is dilute
Bacterium number is interpreted into as 1 × 106~1 × 106The bacterium solution of cfu/mL；(2) it is loaded：By appropriate bacterium solution and 1g high hydroscopic resins, 70mL PBS
Buffer solution, which is added in 250mL triangular flasks (triangular flask sterilizes in advance), makes the concentration of bacterium solution be 1 × 104~2 × 104cfu/mL；
(3) concussion contact：Above-mentioned triangular flask is shaken into 1h at 37 DEG C with the speed of 220r/min；(4) cultivate：Take the suspension after concussion
Liquid 0.5mL is added in the sterile petri dish of diameter 9cm, and each suspension is inoculated with 3 culture dishes, adds about 18mL and melts in advance
Postcooling gently shakes rapidly mixing, lies against on platform, treat the culture medium condensation in culture dish to 45 DEG C of agar medium
Afterwards, culture dish is overturn, makes bottom upward, culture 48h in 37 DEG C of insulating boxs is placed in and counts bacterium colony；(5) compare：Set in experiment homogeneity without
The high hydroscopic resin of antibiotic property is control sample；(6) bacteriostasis rate is calculated：Above-mentioned experiment in triplicate, is averaged and according to following formula meter
Calculate bacteriostasis rate：
Bacteriostasis rate=[(A-B)/A] × 100%,
In formula：A is control sample average colony number；B is antibacterial sample average colony number.
Testing result is shown in Table 1.
Table 1
Odor detection
5g hydroscopic high-molecular resin particles are taken out from each sample, are respectively put into the sealing bottle for filling 150mL urines
The inside, the bottle of sealing, which is placed into 37 DEG C of water-bath, to be heated half an hour, proceeds by survey by five smell evaluation and test persons immediately
Fixed, smell judge is divided into 6 grades, and 1=frees from extraneous odour, 2=slightly smells, 3=is flavoursome but does not stimulate, and 4=has stimulation gas
Taste, 5=strong impulse smells, the intolerable tastes of 6=, each tester respectively make smell assessment, and last is flat
Average is testing result.Testing result is shown in Table 2.
Table 2
Tea polyphenols are not contained in comparison sample 1, comparison sample 2, anti-microbial property is poor, can not also adsorb peculiar smell.It uses
Hygienic articles made from this high hydroscopic resin particle need the stringent sterilizing that carries out that can put goods on the market, and hygienic articles
Do not have the function of eliminating peculiar smell also.It compares and contains tea polyphenols in sample 3 and comparison sample 4, but the water imbibition of comparison sample 3,
Water-retaining property, infiltration rate and logical liquid speed degree are slightly poor；Although sample 4 is compared with prominent water imbibition, due to its preparation method
Part or all of tea polyphenols are wrapped in the inside of the three-dimensional net structure of resin, antibacterial and the performance of absorption peculiar smell are subject to one
Determine the influence of degree.By Comprehensive Correlation as can be seen that utilizing macromolecule water uptake tree made from preparation method provided by the invention
The indices of fat particle are in industry top standard, have excellent water imbibition, water-retaining property, infiltration rate and logical liquid speed
Degree, can meet the requirement of the hygienic articles such as baby paper diaper, adult diaper, female sanitary towel or feminine hygiene pads.More
For importantly, also there is excellent antibiotic property using hydroscopic high-molecular resin particle made from preparation method provided by the invention
Can and absorption peculiar smell function, make its comprehensive performance more excellent, adding in the high hydroscopic resins of tea polyphenols, not only bacteriostasis is big
Big enhancing, such as it is apparent to staphylococcus, Escherichia coli, hay bacillus inhibitory action, can also adsorb peculiar smell has centainly
Deodorization, the hydroscopic high-molecular resin particle obtained with the method are more suitable for applying in the health such as high-end paper diaper and sanitary napkin
Articles for use field.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent substitution to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical solution spirit and
Scope.
Claims (10)
1. the preparation method of a kind of tea polyphenols/high hydroscopic resin particle, which is characterized in that the preparation method includes following step
Suddenly：
(1) 200~300 parts by weight of acrylic acid are dissolved, is configured to the acrylic acid solution that concentration is 20~60wt%, then uses alkali
Property substance adjusts the pH of acrylic acid solution to 6~7；
(2) 2~6 parts by weight of crosslinking agent are added in into acrylic acid solution, add in 0.5~2 parts by weight initiator after mixing, are mixed
It closes solution and polymerisation occurs under the initiation of initiator；After polymerisation, 30~80 purposes are made in obtained colloid
Resin particle；
(3) 100 parts by weight resin particles and 1~3 parts by weight inert inorganic salt powder are uniformly mixed, add 0.5~1.5 weight
Part tea polyphenols and the surface-crosslinked liquid of 20~25 parts by weight are measured, is uniformly mixed, then protects mixture at 150~190 DEG C
Temperature processing, so as to obtain tea polyphenols/high hydroscopic resin particle.
2. preparation method according to claim 1, which is characterized in that in step (3), the inert inorganic salt powder choosing
Any one of autoxidation calcium, kaolin, silica, aluminum sulfate, aluminium oxide, calcium carbonate and magnesium carbonate are a variety of.
3. preparation method according to claim 1, which is characterized in that in step (3), the surface-crosslinked liquid is selected from more
Any one of first alcohol compound, polyhydric amine compounds, epoxide are a variety of；
Preferably, the multicomponent alcoholics compound is selected from any one of ethylene glycol, butanediol, glycerine, triethylene glycol or more
Kind；The polynary aminated compounds is selected from any one of ethylenediamine, diethylene triamine, triethylenediamine or a variety of；And/or the ring
Oxygen compound appointing in butanediol diglycidyl ether, polyglycerol polyglycidyl ether, sorbierite polyglycidyl ether
It is one or more.
4. preparation method according to claim 1, which is characterized in that in step (3), tea polyphenols used are food
Grade, purity is more than 99%.
5. preparation method according to claim 1, which is characterized in that in step (2), the crosslinking agent is selected from N, and N- is sub-
Any in methyl diacrylamine, N hydroxymethyl acrylamide, tetraallyloxyethane, trimethylolpropane tris propylene acid esters
Kind is a variety of；And/or
The initiator is redox initiator, includes Oxidizing and Reducing Agents；The oxidant be selected from benzoyl peroxide,
Any one of isopropyl benzene hydroperoxide, potassium peroxydisulfate, it is sub- that the reducing agent is selected from two hydration sodium bisulphite formaldehydes, sulfuric acid
Any one of iron, sodium hydrogensulfite；Preferably, the reductant-oxidant is potassium peroxydisulfate and sodium hydrogensulfite.
6. preparation method according to claim 1, which is characterized in that in step (2), at 5~15 DEG C described in initiation
Polymerisation；Preferably, the polymerisation is triggered at 8~10 DEG C.
7. preparation method according to claim 1, which is characterized in that in step (2), the resin particle is according to as follows
It is prepared by method：
Micelle is made by being granulated in colloid, then dries micelle obtained at 120~150 DEG C, then by the glue after drying
Grain is ground into particle, and particle is sieved, so as to which the resin particle of 30~80 mesh be made.
8. a kind of tea polyphenols/high hydroscopic resin particle, which is characterized in that using any one of claim 1 to 7 preparation method
It is made.
9. tea polyphenols according to claim 8/high hydroscopic resin particle, which is characterized in that the tea polyphenols/super absorbent resin
The antibiotic rate of fat particle is more than 97%.
10. tea polyphenols/application of the high hydroscopic resin particle in hygienic articles described in claim 8 or 9；The hygienic articles
For any one of paper diaper, sanitary napkin, panty liner.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109535495A (en) * | 2018-11-13 | 2019-03-29 | 浙江金晟环保股份有限公司 | Biodegradable water-absorbent material of biocidal property for chilled food and preparation method thereof |
| CN110258173A (en) * | 2019-05-05 | 2019-09-20 | 苏州恒康新材料有限公司 | Height water conservation antibiotic property paper aid and preparation method thereof |
| CN111228042A (en) * | 2020-01-20 | 2020-06-05 | 雀氏（福建）实业发展有限公司 | Preparation method of odor-removing core body |
| CN111302575A (en) * | 2019-10-22 | 2020-06-19 | 袁国明 | Coagulant, preparation method and application thereof |
| CN113456354A (en) * | 2021-06-30 | 2021-10-01 | 江苏三笑集团有限公司 | Tea polyphenol bacteriostatic odor-removing high-polymer strong-adsorption sanitary towel and preparation method thereof |
| CN113558871A (en) * | 2021-07-28 | 2021-10-29 | 诺宸股份有限公司 | Adult paper diaper |
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| CN103588924A (en) * | 2013-11-12 | 2014-02-19 | 华中农业大学 | Tea polyphenol-acrylic acid series super absorbent resin and preparation method thereof |
| CN103665411A (en) * | 2012-09-24 | 2014-03-26 | 浙江卫星石化股份有限公司 | High salt tolerance and high water absorption rate super absorbent resin and preparation method thereof |
| CN107474170A (en) * | 2017-08-15 | 2017-12-15 | 山东诺尔生物科技有限公司 | A kind of preparation method of the high hydroscopic resin of anti-moisture absorption conglomeration |
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| CN103665411A (en) * | 2012-09-24 | 2014-03-26 | 浙江卫星石化股份有限公司 | High salt tolerance and high water absorption rate super absorbent resin and preparation method thereof |
| CN103588924A (en) * | 2013-11-12 | 2014-02-19 | 华中农业大学 | Tea polyphenol-acrylic acid series super absorbent resin and preparation method thereof |
| CN107474170A (en) * | 2017-08-15 | 2017-12-15 | 山东诺尔生物科技有限公司 | A kind of preparation method of the high hydroscopic resin of anti-moisture absorption conglomeration |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109535495A (en) * | 2018-11-13 | 2019-03-29 | 浙江金晟环保股份有限公司 | Biodegradable water-absorbent material of biocidal property for chilled food and preparation method thereof |
| CN110258173A (en) * | 2019-05-05 | 2019-09-20 | 苏州恒康新材料有限公司 | Height water conservation antibiotic property paper aid and preparation method thereof |
| CN111302575A (en) * | 2019-10-22 | 2020-06-19 | 袁国明 | Coagulant, preparation method and application thereof |
| CN111228042A (en) * | 2020-01-20 | 2020-06-05 | 雀氏（福建）实业发展有限公司 | Preparation method of odor-removing core body |
| CN111228042B (en) * | 2020-01-20 | 2021-08-20 | 雀氏（福建）实业发展有限公司 | Preparation method of odor-removing core body |
| CN113456354A (en) * | 2021-06-30 | 2021-10-01 | 江苏三笑集团有限公司 | Tea polyphenol bacteriostatic odor-removing high-polymer strong-adsorption sanitary towel and preparation method thereof |
| CN113558871A (en) * | 2021-07-28 | 2021-10-29 | 诺宸股份有限公司 | Adult paper diaper |
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