CN105602006A - Antibacterial masterbatch for shoe materials and preparation method of antibacterial masterbatch - Google Patents
Antibacterial masterbatch for shoe materials and preparation method of antibacterial masterbatch Download PDFInfo
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- CN105602006A CN105602006A CN201610040349.7A CN201610040349A CN105602006A CN 105602006 A CN105602006 A CN 105602006A CN 201610040349 A CN201610040349 A CN 201610040349A CN 105602006 A CN105602006 A CN 105602006A
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- stone flour
- mud stone
- footwear material
- green mud
- antibacterial matrices
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/223—Packed additives
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- 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
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- 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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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- 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
- C08K5/54—Silicon-containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The invention provides antibacterial masterbatch for shoe materials. The antibacterial masterbatch comprises, by weight, 100 parts of antibacterial agent, 0.1-0.6 part of antioxidant, 2-3 parts of heat stabilizer, 4-5 parts of lubricant and 0.5 part of coupling agent. The invention further provides a preparation method of the antibacterial masterbatch. The antibacterial masterbatch has lasting and efficient antibacterial performance and is high in compatibility with the shoe materials.
Description
Technical field:
The present invention relates to a kind of antibacterial matrices, particularly relate to a kind of antibacterial matrices for footwear material andPreparation method.
Background technology:
In-shoe environment is the place of microorganism raised growth breeding, and it is unfavorable that people healthy causedImpact. According to incompletely statistics, in climate in china humid region, nearly 70% adultSuffer from ringworm of the foot disease, especially young student and soldier in various degree. In West Europe, statistics tableBright, there is 20%～50% people standing the misery that foot's disease is brought, this disease is by fungiMicropopulation causes. Will thoroughly solve the ringworm of the foot and the smelly smell of pin, be only not all right by antibacterial deodourizing socks, also to there is the in-shoe environment of corresponding sanitation and hygiene. Footwear material is as the important component part of footwear, itsAntimicrobial treatment, to keeping good air condition in footwear chamber, suppresses microbial growth in footwear, simultaneouslyWhat reduce foot's disease is very important.
For example, publication number is CN103301806A, within open day, is that 2013.05.16, application people are horseThe Chinese patent application in Yushan discloses " a kind of footwear antibacterial deodorant ", relates to particularly a kind of usingIn the powder of sterilization, deodorizing and the flavouring of footwear body, comprise following component in parts by weight: aluminum sulfateAmmonium 15-35 part, benzoic acid 2-3 part, nano composite antibiotic material 15-25 part, spices 10-25 part,Anion material 15-35 part. The footwear antibacterial deodorant of this invention, not only have sterilization, deodorizing,Hidroschesis, clearing damp, the dry effect of maintenance sole, can also discharge fragrance simultaneously, effectively reduced solePeculiar smell. But the problem that this invention exists is: its antimicrobial efficiency is not high, and persistence is not fine,And and footwear material between compatibility poor, cause it easily in footwear material, separate out and lose antibiotic propertyEnergy.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of antibacterial matrices for footwear material, and it has holdsFor a long time efficiently anti-microbial property, and and footwear material between compatibility better.
For solving the problems of the technologies described above, technical scheme of the present invention is:
For an antibacterial matrices for footwear material, comprise the component of following weight portion: 100 parts of antiseptics,0.1～0.6 part, antioxidant, 2～3 parts of heat stabilizers, 4～5 parts of lubricants, 0.5 part of coupling agent;Wherein, the preparation method of antiseptic is:
(1) chlorite is pulverized with pulverizer, proceeding in ball mill ball milling, to obtain average grain diameter be 75The green mud stone flour of μ m, it is in 20% hydrochloric acid solution that green mud stone flour is added to mass concentration, is heated toAfter 80 DEG C, water bath with thermostatic control is stirred after 2 hours and is left standstill 12 hours, after taking out, filtering with deionized water repeatedlyWashing, obtains acidifying green mud stone flour after oven dry;
(2) step (1) gained acidifying green mud stone flour being added to mass concentration is that 10% sodium chloride is moltenIn liquid, be heated to 45 DEG C of constant temperature and stir vibration 10 hours, after taking out, filtering with deionized water repeatedlyWashing, obtains sodium green mud stone flour after oven dry;
(3) step (2) gained sodium green mud stone flour being added to molar concentration is 0.05mol/L, phValue is, in 5 liquor argenti nitratis ophthalmicus, to be heated to 80 DEG C of back flow reaction 4.5 hours, after taking-up, leaks with coreBucket filters, with deionized water cyclic washing in the supernatant liquor of filtrate without silver ion, be placed in vacuum dryIn dry case at 80 DEG C dry 8 hours, proceed to and in tube furnace, be warming up to 300 DEG C of roastings and obtain after 4 hoursCarry silver-colored green mud stone flour;
(4) Si-69 is added in absolute ethyl alcohol, ultrasonic dispersion obtains mass concentration and is after 2 hours2% modified solution, carries silver-colored green mud stone flour by step (3) gained and adds in modified solution, is heated to50 DEG C of stirring and refluxing left standstill 12 hours after 1 hour, after taking out, filtering, used deionized water cyclic washing,Be placed at 80 DEG C of air dry ovens and be dried to constant weight, after grinding, cross 200 mesh sieves, obtain antiseptic.
Preferably, antioxidant of the present invention is antioxidant 1010 or irgasfos 168.
Preferably, heat stabilizer of the present invention is zinc stearate.
Preferably, lubricant of the present invention is silicone powder.
Preferably, coupling agent of the present invention is silane coupler.
Preferably, in step of the present invention (1), the weight ratio of green mud stone flour and hydrochloric acid solution is1:15。
Preferably, in step of the present invention (2), the weight of acidifying green mud stone flour and sodium chloride solutionThan being 1:10.
Preferably, in step of the present invention (3), the weight of sodium green mud stone flour and liquor argenti nitratis ophthalmicusThan being 1:10.
Preferably, in step of the present invention (4), the weight ratio of carrying silver-colored green mud stone flour and Si-69 is15:1。
Another technical problem that the present invention will solve is to provide the preparation of the above-mentioned antibacterial matrices for footwear materialMethod.
For solving the problems of the technologies described above, technical scheme is:
Take by weight each component, each component added in mixer, be heated to 90 DEG C after mixEvenly, then proceed in double screw extruder and melt extrude and obtain extruded stock, the spiral shell of double screw extruderThe draw ratio of bar is 42:1, and feeding section temperature is 140-150 DEG C, and transportation section temperature is150-155 DEG C, melt zone temperature is 160-170 DEG C, head temperature is 160-165 DEG C, by extruded stockAdd granulator granulation, obtain the antibacterial matrices for footwear material after being cooled to room temperature.
Therefore compared with prior art, the present invention has following beneficial effect:
1, chlorite is a kind of layer silicate mineral, has stronger adsorptivity and cation exchangeAbility, silver has very excellent anti-microbial property, almost all can produce and suppress to do all bacteriumsWith, and the silver of minute quantity can reach the effect of kill bacteria, and harmless, persistence is veryBy force, the present invention first by hydrochloric acid to chlorite acidifying, make it occur loose structure, improve its energy of adsorptionPower, then by sodium chloride, sodium ion is introduced between the lamella of chlorite, then react logical with silver nitrateCross ion exchange sodium ion is replaced into silver ion, after roasting, be decomposed into crystallization silver and be carried onBetween the lamella of chlorite, become and carry a silver-colored green mud stone flour, then carry out surface by coupling agent Si-69 and changeProperty, Si-69, becomes its surperficial hydrophily in carrying silver-colored green mud stone flour surface by chemical bond joiningBecome lipophile, the intramolecular organic segment of Si-69 can be carried high silver supported green mud stone flour and footwear material base simultaneouslyThe interface combination of body, effectively improves compatibility between the two, makes to carry silver-colored green mud stone flour and can not analyseGo out, can give full play to silver-colored anti-microbial property after making an addition to footwear material, finally by antioxidant, thermally-stabilisedThe antibacterial matrices that agent, lubricant, coupling agent make has the anti-microbial property of persistent high efficiency, and and footwearCompatibility between material is better;
2, when the antioxidant in antibacterial matrices makes high temperature process that it is applied to footwear material, be not easy xanthochromia; ProfitLubrication prescription can effectively improve mobility and the interior lubricity of antibacterial matrices in the time of application footwear material, thereby improves itStability in footwear material; The existence of coupling agent can further improve the phase between antibacterial matrices and footwear materialCapacitive.
Detailed description of the invention:
Describe the present invention in detail below in conjunction with specific embodiment, in this schematic enforcement of the present inventionExample and explanation are used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1
For the antibacterial matrices of footwear material, comprise the component of following weight portion: 100 parts of antiseptics, antioxygen1680.1 parts of agent, 3 parts of zinc stearates, silicone divides 4.4 parts, 0.5 part of silane coupler.
This preparation method who is used for the antibacterial matrices of footwear material is:
(1) chlorite is pulverized with pulverizer, proceeding in ball mill ball milling, to obtain average grain diameter be 75The green mud stone flour of μ m, it is in 20% hydrochloric acid solution that green mud stone flour is added to mass concentration, chloriteThe weight ratio of powder and hydrochloric acid solution is 1:15, be heated to 80 DEG C after water bath with thermostatic control stir after 2 hours and leave standstill12 hours, after taking out, filtering, use deionized water cyclic washing, after oven dry, obtain acidifying chloritePowder;
(2) step (1) gained acidifying green mud stone flour being added to mass concentration is that 10% sodium chloride is moltenIn liquid, the weight ratio of acidifying green mud stone flour and sodium chloride solution is 1:10, is heated to 45 DEG C of constant temperature and stirsMix vibration 10 hours, after taking out, filtering, use deionized water cyclic washing, after oven dry, obtain sodium greenMudstone powder;
(3) step (2) gained sodium green mud stone flour being added to molar concentration is 0.05mol/L, phValue is that in 5 liquor argenti nitratis ophthalmicus, the weight ratio of sodium green mud stone flour and liquor argenti nitratis ophthalmicus is 1:10, addsHeat, to 80 DEG C of back flow reaction 4.5 hours, is filtered with sand core funnel after taking-up, repeatedly washes by deionized waterWash in the supernatant liquor of filtrate without silver ion, be placed at 80 DEG C of vacuum drying chambers dry 8 hours,Proceed to and in tube furnace, be warming up to 300 DEG C of roastings and after 4 hours, obtain carrying a silver-colored green mud stone flour;
(4) Si-69 is added in absolute ethyl alcohol, ultrasonic dispersion obtains mass concentration and is after 2 hours2% modified solution, carries silver-colored green mud stone flour by step (3) gained and adds in modified solution, carries silver-colored green mudThe weight ratio of stone flour and Si-69 is 15:1, is heated to 50 DEG C of stirring and refluxing and after 1 hour, leaves standstill 12 littleTime, after taking out, filtering, use deionized water cyclic washing, be placed at 80 DEG C of air dry ovens and be driedTo constant weight, after grinding, cross 200 mesh sieves, obtain antiseptic;
(5) take by weight each component, each component is added in mixer, be heated to after 90 DEG CMix, then proceed in double screw extruder and melt extrude and obtain extruded stock, double screw extruderThe draw ratio of screw rod be 42:1, feeding section temperature is 140-150 DEG C, transportation section temperature is150-155 DEG C, melt zone temperature is 160-170 DEG C, head temperature is 160-165 DEG C, by extruded stockAdd granulator granulation, obtain the antibacterial matrices for footwear material after being cooled to room temperature.
Embodiment 2
For the antibacterial matrices of footwear material, comprise the component of following weight portion: 100 parts of antiseptics, antioxygen10100.3 parts of agent, 2.4 parts of zinc stearates, silicone divides 4 parts, 0.5 part of silane coupler.
This preparation method of antibacterial matrices who is used for footwear material is with embodiment 1.
Embodiment 3
For the antibacterial matrices of footwear material, comprise the component of following weight portion: 100 parts of antiseptics, antioxygen10100.5 parts of agent, 2.8 parts of zinc stearates, silicone divides 4.8 parts, 0.5 part of silane coupler.
This preparation method of antibacterial matrices who is used for footwear material is with embodiment 1.
Embodiment 4
For the antibacterial matrices of footwear material, comprise the component of following weight portion: 100 parts of antiseptics, antioxygen1680.2 parts of agent, 2.5 parts of zinc stearates, silicone divides 5 parts, 0.5 part of silane coupler.
This preparation method of antibacterial matrices who is used for footwear material is with embodiment 1.
Embodiment 5
For the antibacterial matrices of footwear material, comprise the component of following weight portion: 100 parts of antiseptics, antioxygen10100.4 parts of agent, 2.7 parts of zinc stearates, silicone divides 4.2 parts, 0.5 part of silane coupler.
This preparation method of antibacterial matrices who is used for footwear material is with embodiment 1.
Embodiment 6
For the antibacterial matrices of footwear material, comprise the component of following weight portion: 100 parts of antiseptics, antioxygen1080.6 parts of agent, 2 parts of zinc stearates, silicone divides 4.5 parts, 0.5 part of silane coupler.
This preparation method of antibacterial matrices who is used for footwear material is with embodiment 1.
The anti-microbial property that embodiment 1-6 and comparative example are made an addition to after footwear material is tested respectively:
Comparative example is that publication number is the Chinese patent of CN103301806A,
Method of testing is: the PVC powder that is 19:1 by weight ratio and embodiment 1-6 or comparative example are putEnter in banbury at 165 DEG C banburying 5 minutes, then put into injection machine 170-190 DEG C of injection moulding compressing tablet,Obtain PVC footwear material sample, test the antimicrobial efficiency of each PVC footwear material sample to various thalline (result asShown in table 1) and place the antimicrobial efficiency (result is as shown in table 2) to various thalline after 180 days.
Table 1
Table 2
Can be found out by table 1 and table 2, embodiment of the present invention 1-6 is all obvious to the antimicrobial efficiency of each thallineHigher than comparative example, and the antimicrobial efficiency decline of placement after 180 days is not obvious, and comparative example is antibacterialEfficiency declines a lot, shows that antimicrobial efficiency of the present invention is higher, and persistence is better, with the phase of footwear materialCapacitive is also better.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting thisBright. Any person skilled in the art scholar all can be under spirit of the present invention and category, to above-mentionedEmbodiment modifies or changes. Therefore, have in technical field under such as and conventionally know that the knowledgeable is notDepart from all equivalences that complete under disclosed spirit and technological thought and modify or change, stillShould be contained by claim of the present invention.
Claims (10)
1. for an antibacterial matrices for footwear material, it is characterized in that: the group that comprises following weight portionPart: 100 parts of antiseptics, 0.1～0.6 part, antioxidant, 2～3 parts of heat stabilizers, lubricant 4～5Part, 0.5 part of coupling agent; Wherein, the preparation method of antiseptic is:
(1) chlorite is pulverized with pulverizer, proceeding in ball mill ball milling, to obtain average grain diameter be 75The green mud stone flour of μ m, it is in 20% hydrochloric acid solution that green mud stone flour is added to mass concentration, is heated toAfter 80 DEG C, water bath with thermostatic control is stirred after 2 hours and is left standstill 12 hours, after taking out, filtering with deionized water repeatedlyWashing, obtains acidifying green mud stone flour after oven dry;
(2) step (1) gained acidifying green mud stone flour being added to mass concentration is 10% sodium chloride solutionIn, be heated to 45 DEG C of constant temperature and stir vibration 10 hours, after taking out, filtering, repeatedly wash by deionized waterWash, after oven dry, obtain sodium green mud stone flour;
(3) step (2) gained sodium green mud stone flour being added to molar concentration is 0.05mol/L, phValue is, in 5 liquor argenti nitratis ophthalmicus, to be heated to 80 DEG C of back flow reaction 4.5 hours, after taking-up, leaks with coreBucket filters, with deionized water cyclic washing in the supernatant liquor of filtrate without silver ion, be placed in vacuum dryIn dry case at 80 DEG C dry 8 hours, proceed to and in tube furnace, be warming up to 300 DEG C of roastings and obtain after 4 hoursCarry silver-colored green mud stone flour;
(4) Si-69 is added in absolute ethyl alcohol, ultrasonic dispersion obtains mass concentration after 2 hours be 2%Modified solution, step (3) gained is carried to silver-colored green mud stone flour and adds in modified solution, be heated to 50 DEG CStirring and refluxing left standstill 12 hours after 1 hour, after taking out, filtering, used deionized water cyclic washing, was placed inIn air dry oven, at 80 DEG C, be dried to constant weight, after grinding, cross 200 mesh sieves, obtain antiseptic.
2. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteStating antioxidant is antioxidant 1010 or irgasfos 168.
3. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteStating heat stabilizer is zinc stearate.
4. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteStating lubricant is silicone powder.
5. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteStating coupling agent is silane coupler.
6. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteState in step (1), the weight ratio of green mud stone flour and hydrochloric acid solution is 1:15.
7. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteState in step (2), the weight ratio of acidifying green mud stone flour and sodium chloride solution is 1:10.
8. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteState in step (3), the weight ratio of sodium green mud stone flour and liquor argenti nitratis ophthalmicus is 1:10.
9. a kind of antibacterial matrices for footwear material according to claim 1, is characterized in that: instituteState in step (4), the weight ratio of carrying silver-colored green mud stone flour and Si-69 is 15:1.
10. according to the system of a kind of antibacterial matrices for footwear material described in claim 1～9 any onePreparation Method, is characterized in that: take by weight each component, each component is added in mixer, addHeat mixes after 90 DEG C, then proceeds in double screw extruder and melt extrudes and obtain extruded stock, twoThe draw ratio of the screw rod of screw extruder is 42:1, and feeding section temperature is 140-150 DEG C, transportation section temperatureDegree is 150-155 DEG C, and melt zone temperature is 160-170 DEG C, and head temperature is 160-165 DEG C, will squeezeDischarging adds granulator granulation, obtains the antibacterial matrices for footwear material after being cooled to room temperature.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610040349.7A CN105602006A (en) | 2016-01-21 | 2016-01-21 | Antibacterial masterbatch for shoe materials and preparation method of antibacterial masterbatch |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610040349.7A CN105602006A (en) | 2016-01-21 | 2016-01-21 | Antibacterial masterbatch for shoe materials and preparation method of antibacterial masterbatch |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660114A (en) * | 2012-05-23 | 2012-09-12 | 福建越特新材料科技有限公司 | Preparation method of plastic antibacterial agent |
| CN104262854A (en) * | 2014-10-22 | 2015-01-07 | 苏州市景荣科技有限公司 | Antibacterial polyvinyl chloride sole material and preparation method thereof |
-
2016
- 2016-01-21 CN CN201610040349.7A patent/CN105602006A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660114A (en) * | 2012-05-23 | 2012-09-12 | 福建越特新材料科技有限公司 | Preparation method of plastic antibacterial agent |
| CN104262854A (en) * | 2014-10-22 | 2015-01-07 | 苏州市景荣科技有限公司 | Antibacterial polyvinyl chloride sole material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 宋胥晨等: "《农业生产资料矿产原料》", 30 September 2013, 化学工业出版社 * |
| 宫雪: ""载纳米银抗菌复合材料的研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 齐贵亮: "《塑料压延成型实用技术》", 31 December 2012, 机械工业出版社 * |
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