CN107312228A - It is a kind of for antibacterial matrices of vinyon and preparation method thereof - Google Patents
It is a kind of for antibacterial matrices of vinyon and preparation method thereof Download PDFInfo
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- CN107312228A CN107312228A CN201710617746.0A CN201710617746A CN107312228A CN 107312228 A CN107312228 A CN 107312228A CN 201710617746 A CN201710617746 A CN 201710617746A CN 107312228 A CN107312228 A CN 107312228A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- 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
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The present invention relates to a kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antiseptics 5 20%, lubricant 0.5%, coupling agent 0.2%, surplus are high-density polyethylene plastics resin.Antibacterial plastic concentrate of the present invention uses multiple compounds, there is good dispersiveness and compatibility with vinyon resin compounded, it is added to vinyon such as HDPE, LDPE, LLDPE, POE, in the product such as other ethylene copolymers or other polyolefin, both excellent ageing-resistant ability and more preferable mechanical property had been shown, greatly prolong service life, have again and resist common germ, suppress resistance venereal bacteria, high-efficient and lasting is water-fastness, play environment purification, eliminate peculiar smell, self-cleaning health care, it is free from environmental pollution and human body is had no side effect, more health benefits are obtained beneficial to people.
Description
Technical field
The invention belongs to feature field of new materials, and in particular to one kind, which has, to be resisted common germ, suppresses resistance venereal bacteria,
High-efficient and lasting it is water-fastness for antibacterial matrices of vinyon and preparation method thereof.
Background technology
The product that vinyl polymer is made such as non-woven fabrics, textile, other extrusions are molded, and the product such as blowing is with society
Progress, frequency of use more and more higher, species is also more and more.But these products do not have bacteria resistance function, accumulate over a long period
The outer surface of product will become dirty, and be also easy to produce peculiar smell.Especially in crowd massing area, vinyl polymer product is used
Frequency it is very high, easily grow or breed the microorganisms such as various harmful bacterias, mould, virus, as a public propagation source, give
The health care belt of people carrys out larger puzzlement.
In view of above-mentioned factor, in recent years, the antibiotic property scientific research to vinyl polymer plastic product both at home and abroad gradually increases
Many, it is mainly obtained by adding the method for a small amount of antiseptic in common plasticses.Through searching document, current antiseptic is by knot
Structure is broadly divided into single inorganic, organic and natural three big series.Inorganic antiseptic is using metal ions such as silver, copper, zinc as antibacterial
Agent, is made by carrier of the porous, inorganic such as phosphate, bentonite nonmetallic materials, strong with heat resistance, but its is expensive, ring
Protect shortcoming, product not wash resistant, being used for a long time and touch the product containing metal ions such as silver, copper, zinc can be to the liver of human body
Adversely affect.
Organic antibacterial agent includes quaternary ammonium salts, imidazoles, pyridines, organic metal class etc., although sterilization speed is fast, antibacterial
Effect significantly, but is also easy to produce drug resistance, and heat endurance is poor, it is impossible to be implanted into vinyl polymer, and Durability of antimicrobial effect is short, toxicity compared with
Greatly, so as to bring new healthy hidden danger.By comparison, natural antibacterial agent is extracted from plant, animal or biology, its
Wide material sources, cost is low, is enriched with safety non-toxic, nutritive and health protection components, is not likely to produce drug resistance and environmentally friendly etc. excellent
Point, therefore its application and research are increasingly valued by people.But natural antibacterial agent is typically from a kind of plant, animal or biology
Middle extraction is formed, and antimicrobial component is single, and antibacterial range is narrow, its poor compatibility between plastics, there is reunion, scattered unequal
Problem, and antimicrobial component is easily separated out in use, antibacterial effect can not be lasting, also anti-medicine of the easy product germ to it
Property, these antiseptics are to the germ such as methicillin-resistant staphylococcus staphylococcus of drug resistance without effect.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of for antibacterial matrices of vinyon and preparation method thereof,
The antibacterial plastic concentrate uses multiple compounds, has good dispersiveness and compatibility with vinyon resin compounded, is added to
In vinyon such as HDPE, LDPE, LLDPE, POE, the product such as other ethylene copolymers or other polyolefin, both showed excellent
Different ageing-resistant ability and more preferable mechanical property, greatly prolongs service life, has again and resists common germ, suppresses resistance venereal disease
Bacterium, high-efficient and lasting is water-fastness, plays environment purification, eliminates peculiar smell, self-cleaning health care, free from environmental pollution and human body is had no side effect,
More health benefits are obtained beneficial to people.
To achieve these goals, the present invention uses following technical scheme:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 5-20%, lubricant 0.3-0.7%, coupling agent 0.1-0.3%, surplus are high-density polyethylene plastics resin.
Preferably, the coupling agent is microencapsulation silane, the preparation process of the microencapsulation silane is:By poly- second
Enol, beta-schardinger dextrin, water are (1.8-2.2) in mass ratio:(9-11):(88-92) is well mixed, and obtains mixed liquor;By 3- (2,
The oxygen of 3- epoxies third) propyl trimethoxy silicane be added in mixed liquor using rotating speed as 11000-13000 revs/min stir 60-90 seconds,
The mass ratio of wherein 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicanes and mixed liquor is (0.1-0.15):1, emulsified
Liquid;Emulsion is spray-dried, microencapsulation silane is obtained.
Preferably, the lubricant is stearic acid, N, N- ethylene bis-oleamides, N, in N'- ethylene bis stearamides
One or more combination thing.
Preferably, the Unined RM antiseptics count by weight including:10-15 parts of phenols, 1-3 parts of allicins,
2-4 parts of hesperidin methyls, 3-5 parts of glycitins, 5-8 parts of dodecylbenzyl dimethyl ammoniums, 10-15 parts of 2,4,5,6- tetrachloros
Phthalonitrile, 0.3-10 part dispersant and 0.56-22 parts of acrylic acid.
In the technical program, the present invention finds a kind of water insoluble, does not fall off, the load antiseptic activated carbon of long acting antibiotic
Technology.The essence of the technology is complete substitution silver or Nano Silver, and organic antiseptic prescription is combined using one kind.The formula technique by
Several antibacterial agents are combined into a kind of mixing powder, are named as Unined RM.Utilize its water insoluble characteristic, outer bonus point
Powder, reaches the characteristic not fallen off forever after adhesive solidification., should additionally, due to Unined RM " contact " antibacterial
Unined RM antimicrobial powders can reach long acting antibiotic function.
The Antibacterial Mechanism of organic antibacterial agent is mainly combined or and mercapto with the anion of pathogenic microorganism cell membrane surface
Base reaction suppresses the breeding of pathogenic microorganism with this so as to destroy the structure of protein or influence the synthesis of biomembrane.Typically
The mechanism of action of organic antibacterial agent is summarized as in fact:1. protease or other biological activity thing needed for acting on biochemical reaction
Matter;2. act on hereditary material DNA or other hereditary particle structures;3. act on biofilm system or cell membrane.
And the present invention adsorbs the pathogenic microorganism with negative electrical charge from the effect of each material coordinated, microorganism is destroyed
Cell membrane mechanism, makes content leak, and can suppress the effect such as pathogen oxidizing ferment, dehydrogenase;Also it can remove pathogenic microorganism film
In lipid material and make protein denaturation;Also pathogenic microorganism mitosis process is may interfere with, suppresses the formation of spindle, shadow
Ring pathogenic microorganism fission process.
Preferably, the phenols is one kind in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol
Or several compositions.The phenols described in one embodiment of the present invention is by 75-85wt% isopropyl methyls phenol and 15-
25wt% clorofenes are constituted.
Preferably, the dispersant is Sodium Polyacrylate salt form dispersant and/or polycarboxylate sodium's type dispersant.At this
Dispersant described in an embodiment is invented by 60-70wt% Sodium Polyacrylate salt form dispersants and 30-40wt% polycarboxylic acids
Sodium-salt type dispersant.
Preferably, the preparation method of the Unined RM antiseptics is:1) by load weighted phenols, allicin, methyl
Aurantiamarin, glycitin, dodecylbenzyl dimethyl ammonium, 2,4,5,6- tetrachloro phthalonitriles and dispersant, are mixed
In 90-95 DEG C of temperature after conjunction, high-speed stirred 45-50 hours under 500-550mm mercury column reduced pressures;
2) by step 1) load weighted acrylic acid is added in obtained solid powder, in 90-95 DEG C of temperature, 500- after mixing
Mixed at high speed 45-50 hours under 550mm mercury column reduced pressures;Cooling, packed for standby use.
Preparation method described in a kind of preparation method of antibacterial matrices for vinyon comprises the following steps:By above-mentioned
Formula is weighed in high-density polyethylene plastics resin, coupling agent input mixer, is stirred at 200-500r/min, 25-50 DEG C
10-30min, adds premix, stirs 2-10min, is then fed into double screw extruder main feeding hopper, and Unined RM resist
Microbial inoculum is added in side spout, melting extrusion, cooling, granulation at 100-220 DEG C, is made for the production of vinyl polymer plastics
The antibacterial matrices of product.
Preferably, the melt flow rate of the high-density polyethylene plastics resin is MI=20g/10min, 190 DEG C/
2.16kg。
Beneficial effects of the present invention:The present invention is combined into a kind of mixing powder using several antibacterial agents, is named as
Unined RM, using its water insoluble characteristic, additional dispersant reaches the characteristic not fallen off forever after adhesive solidification,
Additionally, due to Unined RM " contact " antibacterial, the Unined RM antimicrobial powders can reach long acting antibiotic function;
Antibacterial plastic concentrate of the present invention uses multiple compounds, has good dispersiveness and phase with vinyon resin compounded
Capacitive, is added to vinyon such as HDPE, LDPE, LLDPE, POE, the product such as other ethylene copolymers or other polyolefin
In, excellent ageing-resistant ability and more preferable mechanical property had both been shown, service life is greatly prolonged, there is anti-common disease again
Bacterium, suppress resistance venereal bacteria, high-efficient and lasting is water-fastness, plays environment purification, eliminates peculiar smell, self-cleaning health care, it is free from environmental pollution and
Human body is had no side effect, more health benefits are obtained beneficial to people.
Embodiment
Below by embodiment, the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material are commercially available or the industry is conventional, following
Method in embodiment, is this area conventional method unless otherwise instructed.
N, N'- ethylene bis stearamide, No. CAS:110-30-5.
High-density polyethylene plastics resin is the high-density polyethylene that Exxon Mobil (ExxonMobil) trade mark is HMA-016
Olefine resin.
Isopropyl methyl phenol, i.e. carvacrol, No. CAS:499-75-2.
The chloro- 2- benzylphenols of clorofene, i.e. 4-, No. CAS:120-32-1.
Allicin, No. CAS:539-86-6.
Hesperidin methyl, No. CAS:11013-97-1.
Glycitin, No. CAS:40246-10-4.
Dodecylbenzyl dimethyl ammonium, dodecyl benzyl dimethyl ammonium chloride, No. CAS:139-07-1.
2,4,5,6- tetrachloro phthalonitriles, i.e. Bravo, No. CAS:1897-45-6.
Sodium Polyacrylate salt form dispersant is Xian Chuan companies of France model PROX A11 Sodium Polyacrylate dipersant.
Polycarboxylate sodium's type dispersant is Guangzhou Guan Zhi new materials Science and Technology Ltd. model OS-5040 polycarboxylic acids sodium
Salt form dispersant.
The acrylic acid that acrylic acid provides for Shandong Kaitai Petrochemical Co., Ltd..
The polyvinyl alcohol for the model 2488 that polyvinyl alcohol provides for Renqiu City Jin Yu Chemical Co., Ltd.s.
The food-grade beta-schardinger dextrin that beta-schardinger dextrin provides for Hebei Lin Kang bio tech ltd.
The model that 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicane provides for Nanjing Luo En silicon materials Co., Ltd
KH-560 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicane.
Granulation experiment:
Embodiment 1:
Vinyon resin, lubricant, coupling agent and Unined antibacterial agent combinations system are mixed and are separately added into main, side
Feeding hopper, the amount of Unined antibacterial agent combination systems is 5.0% according to vinyon resin.In dual-screw pelletizer group
(LD40, diameter 52mm, parallel double-screw) is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, recirculated hot air 100
DEG C drying 30 minutes store.
The Unined RM antiseptics are counted including 10-15 parts of phenols, 1-3 parts of allicins, 2-4 parts of methyl by weight
Aurantiamarin, 3-5 part glycitin, 5-8 parts of dodecylbenzyl dimethyl ammoniums, 10-15 parts of 2,4,5,6- monoethyl diformazans
Nitrile, 0.3-10 part dispersant and 0.56-22 parts of acrylic acid.
The dispersant model A11.
The phenols is one or more of groups in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol
Compound.
The preparation method of the Unined RM antiseptics is:
1) by load weighted phenols, allicin, hesperidin methyl, glycitin, dodecylbenzyl dimethyl ammonium, 2,
4,5,6- tetrachloro phthalonitriles and dispersant, in 90-95 DEG C of temperature after mixing, under 500-550mm mercury column reduced pressures at a high speed
Stirring 48 hours;
2) by step 1) load weighted acrylic acid is added in obtained solid powder, in 90-95 DEG C of temperature, 500- after mixing
Mixed at high speed 48 hours under 550mm mercury column reduced pressures;Cooling, packed for standby use.
Embodiment 2:
Vinyon resin, lubricant, coupling agent and Unined antibacterial agent combinations system are mixed and are separately added into main, side
Feeding hopper, the amount of Unined antibacterial agent combination systems is 10.0% according to vinyon resin.In dual-screw pelletizer group
(LD40, diameter 52mm, parallel double-screw) is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, recirculated hot air 100
DEG C drying 30 minutes store.
The Unined RM antiseptics are counted including 10-15 parts of phenols, 1-3 parts of allicins, 2-4 parts of methyl by weight
Aurantiamarin, 3-5 part glycitin, 5-8 parts of dodecylbenzyl dimethyl ammoniums, 10-15 parts of 2,4,5,6- monoethyl diformazans
Nitrile, 0.3-10 part dispersant and 0.56-22 parts of acrylic acid.
The dispersant model A11.
The phenols is one or more of groups in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol
Compound.
The preparation method of the Unined RM antiseptics is:
1) by load weighted phenols, allicin, hesperidin methyl, glycitin, dodecylbenzyl dimethyl ammonium, 2,
4,5,6- tetrachloro phthalonitriles and dispersant, in 90-95 DEG C of temperature after mixing, under 500-550mm mercury column reduced pressures at a high speed
Stirring 48 hours;
2) by step 1) load weighted acrylic acid is added in obtained solid powder, in 90-95 DEG C of temperature, 500- after mixing
Mixed at high speed 48 hours under 550mm mercury column reduced pressures;Cooling, packed for standby use.
Embodiment 3:
Vinyon resin, lubricant, coupling agent and Unined antibacterial agent combinations system are mixed and are separately added into main, side
Feeding hopper, the amount of Unined antibacterial agent combination systems is 20.0% according to vinyon resin.In dual-screw pelletizer group
(LD40, diameter 52mm, parallel double-screw) is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, recirculated hot air 100
DEG C drying 30 minutes store.
The Unined RM antiseptics are counted including 10-15 parts of phenols, 1-3 parts of allicins, 2-4 parts of methyl by weight
Aurantiamarin, 3-5 part glycitin, 5-8 parts of dodecylbenzyl dimethyl ammoniums, 10-15 parts of 2,4,5,6- monoethyl diformazans
Nitrile, 0.3-10 part dispersant and 0.56-22 parts of acrylic acid.
The dispersant model A11.
The phenols is one or more of groups in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol
Compound.
The preparation method of the Unined RM antiseptics is:
1) by load weighted phenols, allicin, hesperidin methyl, glycitin, dodecylbenzyl dimethyl ammonium, 2,
4,5,6- tetrachloro phthalonitriles and dispersant, in 90-95 DEG C of temperature after mixing, under 500-550mm mercury column reduced pressures at a high speed
Stirring 48 hours;
2) by step 1) load weighted acrylic acid is added in obtained solid powder, in 90-95 DEG C of temperature, 500- after mixing
Mixed at high speed 48 hours under 550mm mercury column reduced pressures;Cooling, packed for standby use.
Injection experiment
The master batch particle obtained in EXPERIMENTAL EXAMPLE 1-3 and contrast silver-ion antibiotic master batch are subjected to injection experiment.
Embodiment 4:
The polyethylene master batch and common polythene that embodiment 2 is obtained are cut into slices by 2:98 ratios are mixed, actual Unined's
Net content is 0.2%.Under the conditions of 180-220 DEG C, 25-35 DEG C of mold temperature is made on 350MT injection machines
4cmx6cmx0.1cm plaques.
Embodiment 5:
The polyethylene master batch and common polythene that embodiment 2 is obtained are cut into slices by 5:95 ratios are mixed, actual Unined's
Net content is 0.50%.Under the conditions of 180-220 DEG C, 25-35 DEG C of mold temperature is made on 350MT injection machines
4cmx6cmx0.1cm plaques.
Embodiment 6:
The polyethylene master batch and common polythene that embodiment 1 is obtained are cut into slices by 10:90 ratios are mixed, actual Unined's
Net content is 1.0%.Under the conditions of 180-220 DEG C, 25-35 DEG C of mold temperature is made on 350MT injection machines
4cmx6cmx0.1cm plaques.
Embodiment 7:
The polyethylene master batch and common polythene that embodiment 1 is obtained are cut into slices by 20:80 ratios are mixed, actual Unined's
Net content is 2.0%.Under the conditions of 180-220 DEG C, 25-35 DEG C of mold temperature is made on 350MT injection machines
4cmx6cmx0.1cm plaques.
Comparative example 1:
Polyethylene and commercially available silver-ion antibiotic master batch are mixed, it is 0.2% that the content of effective silver ion, which compares polyethylene,.
Under the conditions of 180-220 DEG C, 4cmx6cmx0.1cm plaques are made in 25-35 DEG C of mold temperature on 350MT injection machines.
Comparative example 2:
Polyethylene and commercially available silver-ion antibiotic master batch are mixed, it is 0.5% that the content of effective silver ion, which compares polyethylene,.
Under the conditions of 180-220 DEG C, 4cmx6cmx0.1cm plaques are made in 25-35 DEG C of mold temperature on 350MT injection machines.
Comparative example 3:
Polyethylene and commercially available silver-ion antibiotic master batch are mixed, it is 1.0% that the content of effective silver ion, which compares polyethylene,.
Under the conditions of 180-220 DEG C, 4cmx6cmx0.1cm plaques are made in 25-35 DEG C of mold temperature on 350MT injection machines.
Comparative example 4:
Polyethylene and commercially available silver-ion antibiotic master batch are mixed, it is 2.0% that the content of effective silver ion, which compares polyethylene,.
Under the conditions of 180-220 DEG C, 4cmx6cmx0.1cm plaques are made in 25-35 DEG C of mold temperature on 350MT injection machines.
Embodiment 8:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 10%, N, N'- ethylene bis stearamides 0.5%, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane 0.2%, surplus is
High-density polyethylene plastics resin.
A kind of preparation method of antibacterial matrices for vinyon:High-density polyethylene plastics is weighed by above-mentioned formula
In resin, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicanes and N, N'- ethylene bis stearamide input mixer, 300
Rev/min, stir 20min at 40 DEG C, be then fed into double screw extruder (draw ratio 40, diameter 52mm, parallel double-screw) master
In feeding hopper, Unined RM antiseptics are added in side spout, are divided into nine humidity provinces, area's temperature in double screw extruder
For 160 DEG C, two area's temperature are 170 DEG C, and three area's temperature are 210 DEG C, and four area's temperature are 200 DEG C, and five area's temperature are 200 DEG C, 6th area
Temperature is 205 DEG C, and seven area's temperature are 205 DEG C, and eight area's temperature are 205 DEG C, and nine area's temperature are 195 DEG C, and head temperature is 200 DEG C,
Screw speed is 180 revs/min, compound melted by heat, in the case where the screw rod of double screw extruder is promoted, through poroid mouth mold stream
Go out, dried 30 minutes with 100 DEG C of recirculated hot air earnestly into 3 × 3mm cylindrical pellets through stock-cutter after tie rod water cooling,
The antibacterial matrices for vinyon are made.
The Unined RM antiseptics count by weight including:12 parts of isopropyl methyl phenol, 2 parts of allicins, 3 parts
Hesperidin methyl, 4 parts of glycitins, 7 parts of dodecylbenzyl dimethyl ammoniums, 12 parts of 2,4,5,6- tetrachloro phthalonitriles, 5
Part Sodium Polyacrylate salt form dispersant and 15 parts of acrylic acid.
The preparation method of the Unined RM antiseptics is:
1) by load weighted isopropyl methyl phenol, allicin, hesperidin methyl, glycitin, dodecylbenzyl two
Methyl ammonium salt, 2,4,5,6- tetrachloro phthalonitriles and Sodium Polyacrylate salt form dispersant, in 93 DEG C of temperature after mixing,
With 800 revs/min of high-speed stirreds 48 hours under 520mm mercury column reduced pressures, solid powder is obtained;
2) by step 1) acrylic acid is added in obtained solid powder, in 93 DEG C of temperature after mixing, 520mm mercury column decompression bar
With 800 revs/min of mixed at high speed 48 hours under part;Room temperature is cooled to produce.
Embodiment 9:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 10%, N, N'- ethylene bis stearamides 0.5%, coupling agent 0.2%, surplus are high-density polyethylene plastics resin.
A kind of preparation method of antibacterial matrices for vinyon:High-density polyethylene plastics is weighed by above-mentioned formula
In resin, coupling agent and N, N'- ethylene bis stearamide input mixer, 20min is stirred at 300 revs/min, 40 DEG C, then
In the main feeding hopper for sending into double screw extruder (draw ratio 40, diameter 52mm, parallel double-screw), Unined RM antiseptics exist
Side spout is added, and nine humidity provinces are divided into double screw extruder, and area's temperature is 160 DEG C, and two area's temperature are 170 DEG C, three
Area's temperature is 210 DEG C, and four area's temperature are 200 DEG C, and five area's temperature are 200 DEG C, and six area's temperature are 205 DEG C, and seven area's temperature are 205
DEG C, eight area's temperature are 205 DEG C, and nine area's temperature are 195 DEG C, and head temperature is 200 DEG C, and screw speed is 180 revs/min, mixing
Expect melted by heat, in the case where the screw rod of double screw extruder is promoted, flowed out through poroid mouth mold, after tie rod water cooling through stock-cutter earnestly into
3 × 3mm cylindrical pellets, are dried 30 minutes with 100 DEG C of recirculated hot air, are made female for the antibacterial of vinyon
Grain.
The Unined RM antiseptics count by weight including:12 parts of isopropyl methyl phenol, 2 parts of allicins, 3 parts
Hesperidin methyl, 4 parts of glycitins, 7 parts of dodecylbenzyl dimethyl ammoniums, 12 parts of 2,4,5,6- tetrachloro phthalonitriles, 5
Part Sodium Polyacrylate salt form dispersant and 15 parts of acrylic acid.
The preparation method of the Unined RM antiseptics is:
1) by load weighted isopropyl methyl phenol, allicin, hesperidin methyl, glycitin, dodecylbenzyl two
Methyl ammonium salt, 2,4,5,6- tetrachloro phthalonitriles and Sodium Polyacrylate salt form dispersant, in 93 DEG C of temperature after mixing,
With 800 revs/min of high-speed stirreds 48 hours under 520mm mercury column reduced pressures, solid powder is obtained;
2) by step 1) acrylic acid is added in obtained solid powder, in 93 DEG C of temperature after mixing, 520mm mercury column decompression bar
With 800 revs/min of mixed at high speed 48 hours under part;Room temperature is cooled to produce.
The coupling agent is microencapsulation silane, and the preparation process of the microencapsulation silane is:By polyvinyl alcohol, β-ring
Dextrin, water are 2 in mass ratio:10:90 are well mixed, and obtain mixed liquor;By 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon
Alkane is added in mixed liquor using rotating speed as 12000 revs/min and stirred 70 seconds, wherein 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicon
The mass ratio of alkane and mixed liquor is 0.12:1, obtain emulsion;Emulsion is spray-dried, EAT is 180 DEG C, is gone out
Air temperature is 75 DEG C, and hot blast wind speed is 4m3/ min, feeding speed is 40mL/min, and atomizer rotating speed is 300 revs/min, obtains micro-
Encapsulated silane.
Embodiment 10:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 10%, N, N'- ethylene bis stearamides 0.5%, coupling agent 0.2%, surplus are high-density polyethylene plastics resin.
A kind of preparation method of antibacterial matrices for vinyon:High-density polyethylene plastics is weighed by above-mentioned formula
In resin, coupling agent and N, N'- ethylene bis stearamide input mixer, 20min is stirred at 300 revs/min, 40 DEG C, then
In the main feeding hopper for sending into double screw extruder (draw ratio 40, diameter 52mm, parallel double-screw), Unined RM antiseptics exist
Side spout is added, and nine humidity provinces are divided into double screw extruder, and area's temperature is 160 DEG C, and two area's temperature are 170 DEG C, three
Area's temperature is 210 DEG C, and four area's temperature are 200 DEG C, and five area's temperature are 200 DEG C, and six area's temperature are 205 DEG C, and seven area's temperature are 205
DEG C, eight area's temperature are 205 DEG C, and nine area's temperature are 195 DEG C, and head temperature is 200 DEG C, and screw speed is 180 revs/min, mixing
Expect melted by heat, in the case where the screw rod of double screw extruder is promoted, flowed out through poroid mouth mold, after tie rod water cooling through stock-cutter earnestly into
3 × 3mm cylindrical pellets, are dried 30 minutes with 100 DEG C of recirculated hot air, are made female for the antibacterial of vinyon
Grain.
The Unined RM antiseptics count by weight including:12 parts of clorofenes, 2 parts of allicins, 3 parts of methyl orange peels
Glycosides, 4 parts of glycitins, 7 parts of dodecylbenzyl dimethyl ammoniums, 12 parts of 2,4,5,6- tetrachloro phthalonitriles, 5 parts of polypropylene
Acid sodium-salt type dispersant and 15 parts of acrylic acid.
The preparation method of the Unined RM antiseptics is:
1) by load weighted clorofene, allicin, hesperidin methyl, glycitin, dodecylbenzyl dimethyl ammonium,
2,4,5,6- tetrachloro phthalonitriles and Sodium Polyacrylate salt form dispersant, in 93 DEG C of temperature after mixing, 520mm mercury column subtracts
With 800 revs/min of high-speed stirreds 48 hours under the conditions of pressure, solid powder is obtained;
2) by step 1) acrylic acid is added in obtained solid powder, in 93 DEG C of temperature after mixing, 520mm mercury column decompression bar
With 800 revs/min of mixed at high speed 48 hours under part;Room temperature is cooled to produce.
The coupling agent is microencapsulation silane, and the preparation process of the microencapsulation silane is:By polyvinyl alcohol, β-ring
Dextrin, water are 2 in mass ratio:10:90 are well mixed, and obtain mixed liquor;By 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon
Alkane is added in mixed liquor using rotating speed as 12000 revs/min and stirred 70 seconds, wherein 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicon
The mass ratio of alkane and mixed liquor is 0.12:1, obtain emulsion;Emulsion is spray-dried, EAT is 180 DEG C, is gone out
Air temperature is 75 DEG C, and hot blast wind speed is 4m3/ min, feeding speed is 40mL/min, and atomizer rotating speed is 300 revs/min, obtains micro-
Encapsulated silane.
Embodiment 11:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 10%, N, N'- ethylene bis stearamides 0.5%, coupling agent 0.2%, surplus are high-density polyethylene plastics resin.
A kind of preparation method of antibacterial matrices for vinyon:High-density polyethylene plastics is weighed by above-mentioned formula
In resin, coupling agent and N, N'- ethylene bis stearamide input mixer, 20min is stirred at 300 revs/min, 40 DEG C, then
In the main feeding hopper for sending into double screw extruder (draw ratio 40, diameter 52mm, parallel double-screw), Unined RM antiseptics exist
Side spout is added, and nine humidity provinces are divided into double screw extruder, and area's temperature is 160 DEG C, and two area's temperature are 170 DEG C, three
Area's temperature is 210 DEG C, and four area's temperature are 200 DEG C, and five area's temperature are 200 DEG C, and six area's temperature are 205 DEG C, and seven area's temperature are 205
DEG C, eight area's temperature are 205 DEG C, and nine area's temperature are 195 DEG C, and head temperature is 200 DEG C, and screw speed is 180 revs/min, mixing
Expect melted by heat, in the case where the screw rod of double screw extruder is promoted, flowed out through poroid mouth mold, after tie rod water cooling through stock-cutter earnestly into
3 × 3mm cylindrical pellets, are dried 30 minutes with 100 DEG C of recirculated hot air, are made female for the antibacterial of vinyon
Grain.
The Unined RM antiseptics count by weight including:9.6 parts of isopropyl methyl phenol, 2.4 parts of clorofenes, 2
Part allicin, 3 parts of hesperidin methyls, 4 parts of glycitins, 7 parts of dodecylbenzyl dimethyl ammoniums, 12 parts of 2,4,5,6- tetrachloros
Phthalonitrile, 5 parts of Sodium Polyacrylate salt form dispersants and 15 parts of acrylic acid.
The preparation method of the Unined RM antiseptics is:
1) by load weighted isopropyl methyl phenol, clorofene, allicin, hesperidin methyl, glycitin, dodecyl
Benzyl dimethyl ammonium salt, 2,4,5,6- tetrachloro phthalonitriles and Sodium Polyacrylate salt form dispersant, at 93 DEG C after mixing
With 800 revs/min of high-speed stirreds 48 hours under temperature, 520mm mercury column reduced pressures, solid powder is obtained;
2) by step 1) acrylic acid is added in obtained solid powder, in 93 DEG C of temperature after mixing, 520mm mercury column decompression bar
With 800 revs/min of mixed at high speed 48 hours under part;Room temperature is cooled to produce.
The coupling agent is microencapsulation silane, and the preparation process of the microencapsulation silane is:By polyvinyl alcohol, β-ring
Dextrin, water are 2 in mass ratio:10:90 are well mixed, and obtain mixed liquor;By 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon
Alkane is added in mixed liquor using rotating speed as 12000 revs/min and stirred 70 seconds, wherein 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicon
The mass ratio of alkane and mixed liquor is 0.12:1, obtain emulsion;Emulsion is spray-dried, EAT is 180 DEG C, is gone out
Air temperature is 75 DEG C, and hot blast wind speed is 4m3/ min, feeding speed is 40mL/min, and atomizer rotating speed is 300 revs/min, obtains micro-
Encapsulated silane.
Embodiment 12:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 10%, N, N'- ethylene bis stearamides 0.5%, coupling agent 0.2%, surplus are high-density polyethylene plastics resin.
A kind of preparation method of antibacterial matrices for vinyon:High-density polyethylene plastics is weighed by above-mentioned formula
In resin, coupling agent and N, N'- ethylene bis stearamide input mixer, 20min is stirred at 300 revs/min, 40 DEG C, then
In the main feeding hopper for sending into double screw extruder (draw ratio 40, diameter 52mm, parallel double-screw), Unined RM antiseptics exist
Side spout is added, and nine humidity provinces are divided into double screw extruder, and area's temperature is 160 DEG C, and two area's temperature are 170 DEG C, three
Area's temperature is 210 DEG C, and four area's temperature are 200 DEG C, and five area's temperature are 200 DEG C, and six area's temperature are 205 DEG C, and seven area's temperature are 205
DEG C, eight area's temperature are 205 DEG C, and nine area's temperature are 195 DEG C, and head temperature is 200 DEG C, and screw speed is 180 revs/min, mixing
Expect melted by heat, in the case where the screw rod of double screw extruder is promoted, flowed out through poroid mouth mold, after tie rod water cooling through stock-cutter earnestly into
3 × 3mm cylindrical pellets, are dried 30 minutes with 100 DEG C of recirculated hot air, are made female for the antibacterial of vinyon
Grain.
The Unined RM antiseptics count by weight including:9.6 parts of isopropyl methyl phenol, 2.4 parts of clorofenes, 2
Part allicin, 3 parts of hesperidin methyls, 4 parts of glycitins, 7 parts of dodecylbenzyl dimethyl ammoniums, 12 parts of 2,4,5,6- tetrachloros
Phthalonitrile, 5 parts of polycarboxylate sodium's type dispersants and 15 parts of acrylic acid.
The preparation method of the Unined RM antiseptics is:
1) by load weighted isopropyl methyl phenol, clorofene, allicin, hesperidin methyl, glycitin, dodecyl
Benzyl dimethyl ammonium salt, 2,4,5,6- tetrachloro phthalonitriles and polycarboxylate sodium's type dispersant, in 93 DEG C of temperature after mixing
Degree, with 800 revs/min of high-speed stirreds 48 hours under 520mm mercury column reduced pressures, obtains solid powder;
2) by step 1) acrylic acid is added in obtained solid powder, in 93 DEG C of temperature after mixing, 520mm mercury column decompression bar
With 800 revs/min of mixed at high speed 48 hours under part;Room temperature is cooled to produce.
The coupling agent is microencapsulation silane, and the preparation process of the microencapsulation silane is:By polyvinyl alcohol, β-ring
Dextrin, water are 2 in mass ratio:10:90 are well mixed, and obtain mixed liquor;By 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon
Alkane is added in mixed liquor using rotating speed as 12000 revs/min and stirred 70 seconds, wherein 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicon
The mass ratio of alkane and mixed liquor is 0.12:1, obtain emulsion;Emulsion is spray-dried, EAT is 180 DEG C, is gone out
Air temperature is 75 DEG C, and hot blast wind speed is 4m3/ min, feeding speed is 40mL/min, and atomizer rotating speed is 300 revs/min, obtains micro-
Encapsulated silane.
Embodiment 13:
A kind of antibacterial matrices for vinyon, the antibacterial matrices are by weight percentage:Unined RM antibacterials
Agent 10%, N, N'- ethylene bis stearamides 0.5%, coupling agent 0.2%, surplus are high-density polyethylene plastics resin.
A kind of preparation method of antibacterial matrices for vinyon:High-density polyethylene plastics is weighed by above-mentioned formula
In resin, coupling agent and N, N'- ethylene bis stearamide input mixer, 20min is stirred at 300 revs/min, 40 DEG C, then
In the main feeding hopper for sending into double screw extruder (draw ratio 40, diameter 52mm, parallel double-screw), Unined RM antiseptics exist
Side spout is added, and nine humidity provinces are divided into double screw extruder, and area's temperature is 160 DEG C, and two area's temperature are 170 DEG C, three
Area's temperature is 210 DEG C, and four area's temperature are 200 DEG C, and five area's temperature are 200 DEG C, and six area's temperature are 205 DEG C, and seven area's temperature are 205
DEG C, eight area's temperature are 205 DEG C, and nine area's temperature are 195 DEG C, and head temperature is 200 DEG C, and screw speed is 180 revs/min, mixing
Expect melted by heat, in the case where the screw rod of double screw extruder is promoted, flowed out through poroid mouth mold, after tie rod water cooling through stock-cutter earnestly into
3 × 3mm cylindrical pellets, are dried 30 minutes with 100 DEG C of recirculated hot air, are made female for the antibacterial of vinyon
Grain.
The Unined RM antiseptics count by weight including:9.6 parts of isopropyl methyl phenol, 2.4 parts of clorofenes, 2
Part allicin, 3 parts of hesperidin methyls, 4 parts of glycitins, 7 parts of dodecylbenzyl dimethyl ammoniums, 12 parts of 2,4,5,6- tetrachloros
Phthalonitrile, 3.25 parts of Sodium Polyacrylate salt form dispersants, 1.75 parts of polycarboxylate sodium's type dispersants and 15 parts of acrylic acid.
The preparation method of the Unined RM antiseptics is:
1) by load weighted isopropyl methyl phenol, clorofene, allicin, hesperidin methyl, glycitin, dodecyl
Benzyl dimethyl ammonium salt, 2,4,5,6- tetrachloro phthalonitriles, Sodium Polyacrylate salt form dispersant and polycarboxylate sodium's type are scattered
Agent is mixed, and solid is obtained at 93 DEG C of temperature, 520mm mercury column reduced pressures with 800 revs/min of high-speed stirreds 48 hours after mixing
Powder;
2) by step 1) acrylic acid is added in obtained solid powder, in 93 DEG C of temperature after mixing, 520mm mercury column decompression bar
With 800 revs/min of mixed at high speed 48 hours under part;Room temperature is cooled to produce.
The coupling agent is microencapsulation silane, and the preparation process of the microencapsulation silane is:By polyvinyl alcohol, β-ring
Dextrin, water are 2 in mass ratio:10:90 are well mixed, and obtain mixed liquor;By 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon
Alkane is added in mixed liquor using rotating speed as 12000 revs/min and stirred 70 seconds, wherein 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicon
The mass ratio of alkane and mixed liquor is 0.12:1, obtain emulsion;Emulsion is spray-dried, EAT is 180 DEG C, is gone out
Air temperature is 75 DEG C, and hot blast wind speed is 4m3/ min, feeding speed is 40mL/min, and atomizer rotating speed is 300 revs/min, obtains micro-
Encapsulated silane.
Antibacterial test
Antibacterial test is according to ISO22196:2011 standards are carried out.The strain of experiment is Escherichia coli (ATCC8739), resistance to first
Oxygen XiLin golden yellow staphylococcus (ATCC33591), golden yellow staphylococcus (ATCC6538), Candida albicans (ATCC10231), lung
Scorching Klebsiella (ATCC4352).
As a result:
Table 1:The original antibacterial activity value of print
Embodiment 4-7 all shows that antibacterial activity value is above 0.5, illustrates that the present invention has the bacteriostasis of practicality.
Warm water immersion test
An aperture is made a call in one end wherein for obtained print in injection experiment, so as to a glass weight with a cotton thread
Print is tied down, it is possible to be immersed into water.Print is put into 1000ml beaker, about 1000ml distilled water is added, in idol
In the case of your stirring, 50 DEG C +/- 0.5 DEG C is heated the water to, is placed 168 hours;Then the 1000ml distilled water renewed, heating
To 50 DEG C +/- 0.5 DEG C, place 168 hours.The experiment will repeat to continue 4320 hours (180 days).After 180 days, print is taken
Go out, dry, and make antibacterial test.
Table 2:Antibacterial activity value after warm water immersion
It is demonstrated experimentally that being soaked by warm water, the antibacterial activity value of print of the invention has almost no change, it is shown that this hair
Bright practical wash durability.And the antibacterial functions of the sample contrasted are greatly reduced the degree that can not be used.
ES non-woven fabrics is tested:
ES non-woven fabrics practicality commercialities are very strong.Particularly on hygienic material, ES non-woven fabrics is widely used.Test this hair
It is bright in commercial kitchen area, such as have Special Significance on ES non-woven fabrics.Embodiment 2 is further used for non-woven spinning productive experiment.
This experiment is intended to prove one of application field of the present invention.The present invention can be used in other use polyolefin or
In the Application of composite of polyolefine material.The master batch that embodiment 2 is obtained adds HDPE (MI=20g/10min) by 5% weight ratio,
Then after carrying out with PET bicomponent spin again, working process is into chopped fiber, then by working process into ES non-woven fabrics.Nonwoven
The grammes per square metre of cloth is 20.5g/m2.The physical mechanical index of the non-woven fabrics and non-woven fabrics that master batch obtains is not added with without substantial area
Not.Non-woven fabrics carries out carrying out antibacterial test according to standard GB/T20944.3-2008.Here is test result.
Table 3:The bacteriostasis rate test result of non-woven fabrics (according to GB/T20944.3-2008 standards)
From table 3 it can be seen that non-woven fabrics is above 70% to the bacteriostasis rate of the strain of test, meet antibacterial requirement.
Anti-aging experiment:
According to thermo-oxidative ageing experimental standard GB/T7141-2008, to the embodiment 8-13 antibacterial for vinyon
Master batch carries out artificially roughening (90 DEG C, 500h).Specific test result is shown in Table 4.
Table 4:Ageing resistace test table (90 DEG C, 500h)
Stretching strength retentivity, % | Impact strength conservation rate, % | |
Embodiment 8 | 90.8 | 90.5 |
Embodiment 9 | 91.7 | 92.9 |
Embodiment 10 | 91.2 | 93.1 |
Embodiment 11 | 93.1 | 94.6 |
Embodiment 12 | 92.4 | 94.4 |
Embodiment 13 | 95.5 | 96.8 |
Master batch antibacterial tests:
The anti-microbial property of the embodiment 8-13 antibacterial matrices for vinyon is tested, referred to
GB21551.2-2010《The antibacterial of family expenses and similar applications electrical equipment, degerming, purification function anti-biotic material particular/special requirement》Carry out.
Bacterium is used in detection:Escherichia coli ATCC25922 (Escherichia coli).Specific test result is shown in Table 5.
Table 5:Anti-microbial property test table
Escherichia coli sterilizing rate, % | |
Embodiment 8 | 93.7 |
Embodiment 9 | 95.2 |
Embodiment 10 | 94.9 |
Embodiment 11 | 98.8 |
Embodiment 12 | 98.5 |
Embodiment 13 | 99.6 |
Silane is transformed into solid state powder by the embodiment of the present invention 9 using microencapsulation silane, is mixed with integral plastics system
Evenly, it is made more to disperse.
Claims (8)
1. a kind of antibacterial matrices for vinyon, it is characterised in that the antibacterial matrices are by weight percentage:
Unined RM antiseptics 5-20%, lubricant 0.3-0.7%, coupling agent 0.1-0.3%, surplus is high-density polyethylene plastics
Resin.
2. a kind of antibacterial matrices for vinyon according to claim 1, it is characterised in that the lubricant is
One or more combination thing in stearic acid, N, N- ethylene bis-oleamides, N, N'- ethylene bis stearamides.
3. a kind of antibacterial matrices for vinyon according to claim 1, it is characterised in that the coupling agent is
Microencapsulation silane, the preparation process of the microencapsulation silane is:It is in mass ratio by polyvinyl alcohol, beta-schardinger dextrin, water
(1.8-2.2):(9-11):(88-92) is well mixed, and obtains mixed liquor;By 3- (oxygen of 2,3- epoxies third) propyl trimethoxy silicon
Alkane is added in mixed liquor using rotating speed as 11000-13000 revs/min and stirred 60-90 seconds, wherein 3- (2,3- the third oxygen of epoxy) propyl group
The mass ratio of trimethoxy silane and mixed liquor is (0.1-0.15):1, obtain emulsion;Emulsion is spray-dried, obtained
To microencapsulation silane.
4. a kind of antibacterial matrices for vinyon according to claim 1, it is characterised in that the Unined
RM antiseptics are counted yellow including 10-15 parts of phenols, 1-3 portions of allicins, 2-4 portions of hesperidin methyls, 3-5 portions of soya beans by weight
Glycosides, 5-8 parts of dodecylbenzyl dimethyl ammoniums, 10-15 parts of 2,4,5,6- tetrachloro phthalonitriles, 0.3-10 parts of dispersants with
0.56-22 parts of acrylic acid.
5. a kind of antibacterial matrices for vinyon according to claim 4, it is characterised in that the phenols is different
One or more combination thing in hydroxypropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol.
6. a kind of antibacterial matrices for vinyon according to claim 4, it is characterised in that the dispersant is
Sodium Polyacrylate salt form dispersant and/or polycarboxylate sodium's type dispersant.
7. a kind of antibacterial matrices for vinyon according to claim 4 or 5 or 6, it is characterised in that described
The preparation method of Unined RM antiseptics is:
1) by load weighted phenols, allicin, hesperidin methyl, glycitin, dodecylbenzyl dimethyl ammonium, 2,4,5,
6- tetrachloro phthalonitriles and dispersant, in 90-95 DEG C of temperature after mixing, under 500-550mm mercury column reduced pressures at a high speed
Stirring 45-50 hours;
2) by step 1) load weighted acrylic acid is added in obtained solid powder, in 90-95 DEG C of temperature, 500- after mixing
Mixed at high speed 45-50 hours under 550mm mercury column reduced pressures;Cooling, packed for standby use.
8. a kind of preparation method of antibacterial matrices for vinyon as any one of claim 1-7, it is special
Levy and be, comprise the following steps:High-density polyethylene plastics resin, coupling agent and lubricant input are weighed by above-mentioned formula to stir
In machine, 10-30min is stirred at 200-500r/min, 25-50 DEG C, is then fed into double screw extruder main feeding hopper,
Unined RM antiseptics are added in side spout, and melting extrusion, cooling, granulation, are made for polyethylene at 100-220 DEG C
The antibacterial matrices of high molecule plastic product.
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Application publication date: 20171103 |