CN107841795A - A kind of long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths and preparation method thereof - Google Patents
A kind of long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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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
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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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
- 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
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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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
- 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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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths and preparation method thereof, are included in the antibacterial matrices for adding that percentage by weight is 2 5% in non-woven fabrics raw material, non-woven fabrics is prepared by existing process.Antibacterial matrices are added in long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths of the present invention, the antibacterial matrices use 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 and anti-flammability 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 have no side effect to human body, more health benefits are obtained beneficial to people.
Description
Technical field
The invention belongs to feature new material product scope, and in particular to a kind of long acting antibiotic polyethylene ES hot blasts antibacterial without
Spin cloth and preparation method thereof.
Background technology
The products such as such as non-woven fabrics of product made of vinyl polymer, textile, other extrusion injections, blowing are 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 used in crowd massing area, vinyl polymer product
Frequency it is very high, easily grow or breed the microorganisms such as various harmful bacterias, mould, virus, turn into 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
More, 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, it is made using the porous, inorganic nonmetallic materials such as phosphate, bentonite as carrier, it is strong with heat resistance, but its is expensive, ring
Protect shortcoming, product not wash resistant, it is long-term use of 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
Significant effect, but be also easy to produce drug resistance, heat endurance is poor, can not be implanted into vinyl polymer, and Durability of antimicrobial effect is short, toxicity compared with
Greatly, so as to bringing new healthy hidden danger.By comparison, natural antibacterial agent is extracted from plant, animal or biology, its
Wide material sources, cost is low, and there are safe and non-toxic, nutritive and health protection components to enrich, be 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 to extract to form from a kind of plant, animal or biology, and antimicrobial component is single, antibacterial model
Narrow, its poor compatibility between plastics is enclosed, the problems such as reunion, scattered uneven be present, and antimicrobial component is easy in use
Separate out, antibacterial effect can not be lasting, and also easy product germ is to its resistance to the action of a drug, germ of these antiseptics to drug resistance
If methicillin-resistant staphylococcus aureus is without effect.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of long acting antibiotic polyethylene ES hot blasts antibacterial nonwoven cloth and its preparation
Method, the antibacterial matrices of addition use multiple compounds, have well dispersed and compatible with vinyon resin compounded
Property, 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 and anti-flammability had been shown, has greatly prolonged service life, had been had again anti-general
Common fault bacterium, suppress resistance venereal bacteria, high-efficient and lasting is water-fastness, plays environment purification, eliminates peculiar smell, self-cleaning health care, does not pollute ring
Border and have no side effect to human body, more health benefits are obtained beneficial to people.
The invention provides a kind of long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths, the long acting antibiotic polyethylene ES heat
The raw material of wind antibacterial nonwoven cloth includes the antibacterial matrices that percentage by weight is 2-5%.
The antibacterial matrices include the raw material of following weight percentage：Unined RM antiseptics 5-20%, lubricant 0.1-
1%th, coupling agent 0.1-0.5%, surplus are high-density polyethylene plastics resin；
The Unined RM antiseptics include the raw material of following weight parts：Dispersant 0.2-8 parts, acrylic acid 0.56-20.5
Part, phenols 10-15 parts, phellodendron extract 3-5 parts, rue leaf extract 6-10 parts, methyl resveratrol 2-4 parts, glycitin
3-5 parts, 2,4,5,6- tetrachloro phthalonitrile 3-5 parts.
The phenols is one or more of groups in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol
Compound.
The melt flow rate of the high-density polyethylene plastics resin is MI=20g/10min, 190 DEG C/21.6kg of experimental condition.
The lubricant is one kind in expanded graphite, Tissuemat E, butyl stearate.
Preferably, the expanded graphite is the expanded graphite of surface treatment.
Preferably, the lubricant is the expanded graphite and/or butyl stearate of surface treatment.
It is highly preferred that the lubricant is the expanded graphite of surface treatment and the mixture of butyl stearate, the surface
The expanded graphite of processing and the mass ratio of butyl stearate are (2-5)：1.
The coupling agent is prepared by following methods：
(1) by gamma-aminopropyl-triethoxy-silane and cinnamic acid in molar ratio (2-5)：1 mixing, mixture is obtained, then added
Enter the ethanol of 4-6 times of mixture quality, at 20-30 DEG C with 100-200 revs/min of stirring 10-20 minute, obtain mixed solution A；
(2) concentrated sulfuric acid that mass fraction is 98% is added in mixed solution A, then is warming up to 60-80 DEG C, turned with 100-200/
Divide stirring 8-12 hours, obtain solution B, the wherein mass ratio of mixed solution A and the concentrated sulfuric acid is 1:(0.01-0.05)；
(3) mixed solution B has been concentrated under reduced pressure into crystal precipitation under the conditions of pressure is 60Pa, temperature is 40-60 DEG C,
1-3 hours are placed at 10-20 DEG C, with 300 mesh filter-cloth filterings, solid is dried to constant weight in 40-60 DEG C of vacuum drying chamber, is obtained
Coupling agent.
The expanded graphite of the surface treatment is prepared by following methods：
(1) by the concentrated sulfuric acid and mass fraction that mass fraction is 98% be 30% hydrogen peroxide by volume (6-10):1
Mixing, obtains mixed liquor, crystalline flake graphite and mixed liquor is pressed into solid-to-liquid ratio 1g：(3-6) mL is mixed, at 25-35 DEG C with 100-200
Rev/min stirring 60-80 minutes, with 300 mesh filter-cloth filterings, it is 5-7 that solid, which is washed with deionized to water outlet pH, is added in solid
The acetic acid of 2-4 times of crystalline flake graphite quality, at 25-35 DEG C with 100-200 revs/min of stirring 2-3 hour, with 300 mesh filter-cloth filterings, extremely
It is 5-7 that solid, which is washed with deionized to water outlet pH, and solid dries 2-3 hours in 60-70 DEG C of drying box, obtains intercalation stone
Ink；
(2) intercalated graphite is incubated the 20-40 seconds in 700-900 DEG C of Muffle furnace, takes out, obtain expanded graphite；
(3) expanded graphite and mass fraction are pressed into solid-to-liquid ratio 1g for 5-10% sodium dodecyl benzene sulfonate aqueous solution：(5-
10) mL is mixed, and at 40-60 DEG C with 200-300 revs/min of stirring 60-80 minute, using 300 mesh filter-cloth filterings, solid is done in vacuum
With 60-70 DEG C of dry expanded graphite 2-4 hours, being surface-treated in dry case.
The phellodendron extract is prepared by following methods：
(1) water extraction：Golden cypress is cleaned, in 40-50 DEG C of dry 3-5 hour, obtains drying golden cypress, adds and dry golden cypress weight
6-10 times of distilled water, then 40-60 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, filtrate A is obtained, is added in filter residue
Enter the distilled water of dry 4-6 times of golden cypress weight, then 30-40 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, filtered
Liquid B, the distilled water for drying 4-6 times of golden cypress weight is added in filter residue, then 30-40 minutes are incubated at 95-98 DEG C, using the filter of 300 mesh
Cloth filters, and obtains liquor C, merging filtrate A, liquor B, liquor C, it is 1.3-1.35 (50 that relative density is concentrated at 40-60 DEG C
DEG C) concentrate；
(2) volume fraction that 5 times of concentrate weight is added in concentrate is 95% ethanol water, turned with 100-200/
Divide stirring 10-20 minutes, stand 6-14 hours, with 3000-5000 revs/min of centrifugation 5-10 minute, be in pressure by supernatant
60Pa, temperature be concentrated under reduced pressure under the conditions of being 40-60 DEG C recovery ethanol to relative density be 1.3-1.35 (50 DEG C) concentrate, adopt
With 200 mesh filter-cloth filterings, filtrate is dried in vacuo 10-20 hours at 40-60 DEG C, vacuum 60Pa, obtains phellodendron extract.
The rue leaf extract is prepared by following methods：
(1) rue leaf is cleaned, in 40-50 DEG C of dry 3-5 hour, obtains drying rue leaf, add and dry rue leaf weight
6-10 times of distilled water of amount, then in 95-98 DEG C of insulation 40-60 minute, using 300 mesh filter-cloth filterings, filtrate A is obtained, in filter residue
The distilled water for drying 4-6 times of rue leaf weight is added, then 30-40 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, is obtained
To liquor B, the distilled water for drying 4-6 times of rue leaf weight is added in filter residue, then 30-40 minutes are incubated at 95-98 DEG C, use
300 mesh filter-cloth filterings, liquor C is obtained, merging filtrate A, liquor B, liquor C, it is 1.5- that relative density is concentrated at 40-60 DEG C
The concentrate of 1.65 (50 DEG C)；
(2) volume fraction that 4 times of concentrate weight is added in concentrate is 95% ethanol water, turned with 100-200/
Divide stirring 10-20 minutes, stand 6-14 hours, with 3000-5000 revs/min of centrifugation 5-10 minute, be in pressure by supernatant
60Pa, temperature be concentrated under reduced pressure under the conditions of being 40-60 DEG C recovery ethanol to relative density be 1.5-1.65 (50 DEG C) concentrate, adopt
With 200 mesh filter-cloth filterings, filtrate is dried in vacuo 10-20 hours at 40-60 DEG C, vacuum 60Pa, obtains rue leaf extract.
The Unined RM antiseptics are prepared by following methods：
(1) by load weighted phenols, phellodendron extract, rue leaf extract, methyl resveratrol, glycitin, 2,4,
5,6- tetrachloro phthalonitriles, dispersant mix at 20-30 DEG C, in 90-95 DEG C, 500-550mm mercury column reduced pressures after mixing
Under with 300-500 revs/min stirring 40-60 hours, obtain powder；
(2) powder that step (1) obtains is mixed with acrylic acid, depressurized after mixing in 90-95 DEG C, 500-550mm mercury column
Under the conditions of with 300-500 revs/min stirring 40-60 hours.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, 10-30min is stirred at 200-500r/min, 25-50 DEG C, by rotational speed regulation to 600-800r/
Min stirs 2-10min, is then fed into double screw extruder main feeding hopper, and Unined RM antiseptics add in side spout,
In 150-220 DEG C of melting extrusion, cooling, granulation, antibacterial matrices are made.
Present invention also offers a kind of preparation method of long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths, it is included in nonwoven
The antibacterial matrices that percentage by weight is 2-5% are added in cloth raw material, non-woven fabrics is prepared by existing process and obtains.
In the technical program, present invention searching is a kind of not soluble in water, does not fall off, the antiseptic technology of long acting antibiotic.Should
The essence of technology is complete substitution silver or Nano Silver, uses a kind of compound organic antiseptic prescription.The formula technique is by several anti-
Bacterium reagent is combined into a kind of mixing powder, is named as Unined RM, additional dispersant, reaches what is do not fallen off forever after solidification
Characteristic, the 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 biochemical reaction are acted on
Matter；(2) hereditary material DNA or other hereditary particle structures are acted on；(3) biofilm system or cell membrane are acted on.
And the present invention is acted on from each material coordinated, pathogenic microorganism of the absorption with negative electrical charge, 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.
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, additional dispersant, reach the characteristic not fallen off forever after solidification, can reach long acting antibiotic function.
Antibacterial matrices of the present invention use multiple compounds, have good dispersiveness and phase with vinyon resin compounded
Capacitive, it is added to the products such as vinyon such as HDPE, LDPE, LLDPE, POE, other ethylene copolymers or other polyolefin
In, excellent ageing-resistant ability and more preferable mechanical property and anti-flammability had both been shown, has greatly prolonged service life, had been had again anti-
Common germ, suppress resistance venereal bacteria, high-efficient and lasting is water-fastness, plays environment purification, eliminates peculiar smell, self-cleaning health care, does not pollute
Environment and have no side effect to human body, more health benefits are obtained beneficial to people.
Embodiment
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, it is this area conventional method unless otherwise instructed.
High-density polyethylene plastics resin, the trade mark of Dushanzi petrochemical iy produced is used as DMDA-8920 high-density polyethylene
Olefine resin.
Common polythene is cut into slices, and is cut into slices using the polyethylene of Shanghai Hu Zheng Industrial Co., Ltd.s production.
Acrylic acid, No. CAS：79-10-7.The industrial acrylic acid produced using Qilu Petrochemical.
Antiphen, No. CAS：97-23-4.AlfaAesar (China) Chemical Co., Ltd. produces.
Golden cypress, Classification system：Cortex Phellodendri Chinensis, rutaceae wampee
Phellodendron chinenseSchneid. dry bark.
Rue leaf, for the wooden herbaceos perennial rue (Ruta graveolens) of Rutaceae, rue category basal part of stem
Leaf.
Methyl resveratrol, i.e., white reed lamb's-quarters alcohol methylated derivative use (E) -3 in embodiment, and 5,4,-trimethoxy -
1,2- talan, abbreviation BTM-0512, purity 99.5%, lot number：110510, Pharmacy of Xiangye No. 2 Hospital of Central South University.
Glycitin, No. CAS：40246-10-4, the production of lark prestige Science and Technology Ltd..
2,4,5,6- tetrachloro phthalonitriles, No. CAS：1897-45-6.Shanghai Mike's woods biochemical technology Co., Ltd gives birth to
Production.
Tissuemat E, No. CAS：9002-88-4, the model PE520 produced using German Ke Laien.
Butyl stearate, No. CAS：123-95-5, the production of lark prestige Science and Technology Ltd..
Crystalline flake graphite, the natural flake graphite produced using Qingdao Dong Kai graphite Co., Ltd, the mesh of particle diameter 325.
Cinnamic acid, No. CAS：140-10-3, the production of lark prestige Science and Technology Ltd..
Gamma-aminopropyl-triethoxy-silane, No. CAS：919-30-2, the production of AlfaAesar (China) Chemical Co., Ltd..
γ-(methacryloxypropyl) propyl trimethoxy silicane, No. CAS：2530-83-8, Shanghai Mai Ruier chemical technologies
Co., Ltd produces.
VTES, No. CAS：78-08-0, the production of Shanghai Mai Ruier chemical technologies Co., Ltd.
The concentrated sulfuric acid, No. CAS：7664-93-9, the production of Shanghai Zhi Xin Chemical Co., Ltd.s, concentration 98%.
Hydrogen peroxide, No. CAS：7722-84-1, the production of Shanghai Han Hong Science and Technology Co., Ltd., mass fraction 30%.
Acetic acid, No. CAS：64-19-7, the production of lark prestige Science and Technology Ltd..
Neopelex, No. CAS：25155-30-0, the production of Shanghai Mai Ruier chemical technologies Co., Ltd.
Ethanol, No. CAS：64-17-5, Chemical Reagent Co., Ltd., Sinopharm Group's production.
Dispersant, using polyacrylic acid sodium salt, Prox A11 are first created using France in embodiment.
Silver-ion antibiotic master batch, using the silver-ion antibiotic master batch of the micro-nano new material Co., Ltd production of Hangzhou gold, type
Number HFK.
Antibacterial test：According to ISO22196:2011 standards are carried out.The strain of experiment is Escherichia coli (ATCC8739), resistance to
Methicillin staphylococcus aureus (ATCC33591), staphylococcus aureus (ATCC6538), Candida albicans
(ATCC10231), Friedlander's bacillus (ATCC4352).
Warm water immersion test：An aperture is made a call in one end to the print obtained in injection experiment wherein, so as to a glass weight
Thing is tied down print with a cotton thread, and can be immersed into water.Print is put into 1000mL beaker, adds about 1000mL
Distilled water, in the case where stirring once in a while, 50 DEG C are heated the water to, is placed 168 hours；Then the 1000mL distilled water renewed,
50 DEG C are heated to, is placed 168 hours.The experiment will repeat to continue 4320 hours (180 days).After 180 days, print is taken out, dried in the air
It is dry, and make antibacterial test.
Anti-flammability is tested：With reference to GB/T2406.1-2008《Plastics determine burning behavior with oxygen index method》Test sample
Oxygen index (OI).
Embodiment 1
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 5.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is Tissuemat E.
The coupling agent is gamma-aminopropyl-triethoxy-silane.
The antibacterial matrices are prepared by following methods：High-density polyethylene plastics resin, profit are weighed by above-mentioned formula
Lubrication prescription, coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred
6min, it is then fed into double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics
Add, be granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing in side spout, 100 DEG C of recirculated hot air dries 30 points
Clock, antibacterial matrices are made.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 5th area
205 DEG C, 210 DEG C of 6th area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The Unined RM antiseptics are prepared by following methods：
(1) by load weighted antiphen, phellodendron extract, rue leaf extract, methyl resveratrol, glycitin, 2,
4,5,6- tetrachloro phthalonitriles, dispersant mix at 25 DEG C, with 400 under 92 DEG C, 520mm mercury column reduced pressures after mixing
Rev/min stirring 48 hours, obtain powder；
(2) powder that step (1) obtains is mixed with acrylic acid, after mixing under 92 DEG C, 520mm mercury column reduced pressures with
400 revs/min are stirred 48 hours.
The phellodendron extract is prepared by following methods：
(1) water extraction：Golden cypress is cleaned, dried 4 hours at 45 DEG C, obtains drying golden cypress, adds and dry 8 times of golden cypress weight
Distilled water, then 50 minutes are incubated at 96 DEG C, using 300 mesh filter-cloth filterings, filtrate A is obtained, is added in filter residue and dries golden cypress weight 5
Distilled water again, then 35 minutes are incubated at 96 DEG C, using 300 mesh filter-cloth filterings, liquor B is obtained, is added in filter residue and dries golden cypress
The distilled water that 5 times of weight, then 35 minutes are incubated at 96 DEG C, using 300 mesh filter-cloth filterings, obtain liquor C, merging filtrate A, filtrate
B, liquor C, the concentrate that relative density is 1.3 (50 DEG C) is concentrated at 50 DEG C；
(2) volume fraction that 5 times of concentrate weight is added in concentrate is 95% ethanol water, is stirred with 150 revs/min
Mix 15 minutes, stand 10 hours, with 4000 revs/min centrifuge 8 minutes, by supernatant pressure be 60Pa, temperature be 50 DEG C of conditions
Under be concentrated under reduced pressure recovery ethanol to relative density be 1.3 (50 DEG C) concentrate, using 200 mesh filter-cloth filterings, filtrate is at 50 DEG C
Vacuum drying 15 hours, vacuum 60Pa, obtains phellodendron extract.
The rue leaf extract is prepared by following methods：
(1) rue leaf is cleaned, dried 4 hours at 45 DEG C, obtained drying rue leaf, add and dry 8 times of rue leaf weight
Distilled water, then be incubated 50 minutes at 96 DEG C, using 300 mesh filter-cloth filterings, obtain filtrate A, added in filter residue and dry rue leaf
The distilled water that 5 times of weight, then 35 minutes are incubated at 96 DEG C, using 300 mesh filter-cloth filterings, liquor B is obtained, drying is added in filter residue
The distilled water of 5 times of rue leaf weight, then 35 minutes are incubated at 96 DEG C, using 300 mesh filter-cloth filterings, obtain liquor C, merging filtrate
A, liquor B, liquor C, the concentrate that relative density is 1.5 (50 DEG C) is concentrated at 50 DEG C；
(2) volume fraction that 4 times of concentrate weight is added in concentrate is 95% ethanol water, is stirred with 150 revs/min
Mix 15 minutes, stand 10 hours, with 4000 revs/min centrifuge 8 minutes, by supernatant pressure be 60Pa, temperature be 50 DEG C of conditions
Under be concentrated under reduced pressure recovery ethanol to relative density be 1.5 (50 DEG C) concentrate, using 200 mesh filter-cloth filterings, filtrate is at 50 DEG C
Vacuum drying 15 hours, vacuum 60Pa, obtains rue leaf extract.
Embodiment 2
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is Tissuemat E.
The coupling agent is gamma-aminopropyl-triethoxy-silane.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
Embodiment 3
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 20.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is Tissuemat E.
The coupling agent is gamma-aminopropyl-triethoxy-silane.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
Embodiment 4
Antibacterial matrices and the common polythene section in mass ratio 2 that embodiment 2 is obtained:98 ratios mix, and are mixed
Material, actual Unined net content is 0.2%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 area 220
DEG C, 2 220 DEG C of areas, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mould
Have 30 DEG C of temperature, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 5
Antibacterial matrices and the common polythene section in mass ratio 5 that embodiment 2 is obtained:95 ratios mix, and are mixed
Material, actual Unined net content is 0.50%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1st area
220 DEG C, 2 220 DEG C of areas, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 areas 180
DEG C, 30 DEG C of mold temperature, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 6
Antibacterial matrices and the common polythene section in mass ratio 10 that embodiment 2 is obtained:90 ratios mix, and are mixed
Material, actual Unined net content is 1.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 area 220
DEG C, 2 220 DEG C of areas, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mould
Have 30 DEG C of temperature, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 7
Antibacterial matrices and the common polythene section in mass ratio 20 that embodiment 2 is obtained:80 ratios mix, and are mixed
Material, actual Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 area 220
DEG C, 2 220 DEG C of areas, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mould
Have 30 DEG C of temperature, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Comparative example 1
Common polythene section and commercially available silver-ion antibiotic master batch are mixed, obtain compound, the content of effective silver ion
It is 0.2%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2 220 DEG C of areas, 3 215 DEG C of areas,
4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, 30 DEG C of mold temperature, noted in 350MT
4cm × 6cm × 0.1cm plaques are made on molding machine.
Comparative example 2
Common polythene section and commercially available silver-ion antibiotic master batch are mixed, obtain compound, the content of effective silver ion
It is 0.5%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2 220 DEG C of areas, 3 215 DEG C of areas,
4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, 30 DEG C of mold temperature, noted in 350MT
4cm × 6cm × 0.1cm plaques are made on molding machine.
Comparative example 3
Common polythene section and commercially available silver-ion antibiotic master batch are mixed, obtain compound, the content of effective silver ion
It is 1.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2 220 DEG C of areas, 3 215 DEG C of areas,
4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, 30 DEG C of mold temperature, noted in 350MT
4cm × 6cm × 0.1cm plaques are made on molding machine.
Comparative example 4
Common polythene section and commercially available silver-ion antibiotic master batch are mixed, obtain compound, the content of effective silver ion
It is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2 220 DEG C of areas, 3 215 DEG C of areas,
4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, 30 DEG C of mold temperature, noted in 350MT
4cm × 6cm × 0.1cm plaques are made on molding machine.
Embodiment 8
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The coupling agent is gamma-aminopropyl-triethoxy-silane.
The lubricant is butyl stearate.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 9
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is expanded graphite.
The coupling agent is gamma-aminopropyl-triethoxy-silane.
The expanded graphite is prepared by following methods：Crystalline flake graphite is incubated 20- in 700-900 DEG C of Muffle furnace
40 seconds, take out, obtain expanded graphite.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 10
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is the expanded graphite of surface treatment.
The coupling agent is gamma-aminopropyl-triethoxy-silane.
The expanded graphite of the surface treatment is prepared by following methods：
(1) by the concentrated sulfuric acid and mass fraction that mass fraction is 98% be 30% hydrogen peroxide by volume (6-10):1
Mixing, obtains mixed liquor, crystalline flake graphite and mixed liquor is pressed into solid-to-liquid ratio 1g：(3-6) mL is mixed, at 25-35 DEG C with 100-200
Rev/min stirring 60-80 minutes, with 300 mesh filter-cloth filterings, it is 5-7 that solid, which is washed with deionized to water outlet pH, is added in solid
The acetic acid of 2-4 times of crystalline flake graphite quality, at 25-35 DEG C with 100-200 revs/min of stirring 2-3 hour, with 300 mesh filter-cloth filterings, extremely
It is 5-7 that solid, which is washed with deionized to water outlet pH, and solid dries 2-3 hours in 60-70 DEG C of drying box, obtains intercalation stone
Ink；
(2) intercalated graphite is incubated the 20-40 seconds in 700-900 DEG C of Muffle furnace, takes out, obtain expanded graphite；
(3) expanded graphite and mass fraction are pressed into solid-to-liquid ratio 1g for 5-10% sodium dodecyl benzene sulfonate aqueous solution：(5-
10) mL is mixed, and at 40-60 DEG C with 200-300 revs/min of stirring 60-80 minute, using 300 mesh filter-cloth filterings, solid is done in vacuum
With 60-70 DEG C of dry expanded graphite 2-4 hours, being surface-treated in dry case.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 11
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is the expanded graphite of surface treatment.
The coupling agent is prepared by following methods：
(1) by gamma-aminopropyl-triethoxy-silane and cinnamic acid in molar ratio (2-5)：1 mixing, mixture is obtained, then added
Enter the ethanol of 4-6 times of mixture quality, at 20-30 DEG C with 100-200 revs/min of stirring 10-20 minute, obtain mixed solution A；
(2) concentrated sulfuric acid that mass fraction is 98% is added in mixed solution A, then is warming up to 60-80 DEG C, turned with 100-200/
Divide stirring 8-12 hours, obtain solution B, the wherein mass ratio of mixed solution A and the concentrated sulfuric acid is 1:(0.01-0.05)；
(3) mixed solution B has been concentrated under reduced pressure into crystal precipitation under the conditions of pressure is 60Pa, temperature is 40-60 DEG C,
1-3 hours are placed at 10-20 DEG C, with 300 mesh filter-cloth filterings, solid is dried to constant weight in 40-60 DEG C of vacuum drying chamber, is obtained
Coupling agent.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
The preparation method of the expanded graphite of the surface treatment is the same as embodiment 10.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 12
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin, and the actual content of Unined antiseptics is 10.0%.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is the expanded graphite of surface treatment.
The coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
The preparation method of the expanded graphite of the surface treatment is the same as embodiment 10.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 13
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin, and the actual content of Unined antiseptics is 10.0%.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is the expanded graphite of surface treatment.
The coupling agent is VTES.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
The preparation method of the expanded graphite of the surface treatment is the same as embodiment 10.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
Embodiment 14
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin, and the actual content of Unined antiseptics is 10.0%.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant is butyl stearate.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
The preparation method of the coupling agent is the same as embodiment 11.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
The obtained original antibacterial activity value test result of print：Escherichia coli 4.6, methicillin-resistant staphylococcus aureus
4.6, staphylococcus aureus 4.5, Candida albicans 4.5, Friedlander's bacillus 4.3；
Antibacterial activity test result after obtained long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths warm water immersion：Greatly
Enterobacteria 4.5, methicillin-resistant staphylococcus aureus 4.6, staphylococcus aureus 4.6, Candida albicans 4.5, pneumonia gram
The primary Salmonella 4.4 of thunder；
Obtained print oxygen index (OI) test result：31.3%.
Embodiment 15
Antibacterial matrices raw material (percentage by weight)：Unined RM antiseptics 10.0%, lubricant 0.5%, coupling agent
0.2%, surplus is high-density polyethylene plastics resin, and the actual content of Unined antiseptics is 10.0%.
Unined RM antiseptics raw materials (parts by weight)：3 parts of dispersant, 12 parts of acrylic acid, 12 parts of antiphen, golden cypress extraction
4 parts of thing, 8 parts of rue leaf extract, 3 parts of methyl resveratrol, 4 parts of glycitin, 4 parts of 2,4,5,6- tetrachloro phthalonitrile.
The lubricant for surface treatment expanded graphite and butyl stearate mixture, the expansion of the surface treatment
The mass ratio of graphite and butyl stearate is 4：1.
The antibacterial matrices are prepared by following methods：By formula weigh high-density polyethylene plastics resin, lubricant,
Coupling agent, put into mixer, in 300r/min, 35 DEG C of stirring 20min, rotational speed regulation to 700r/min is stirred into 6min, so
It is sent into afterwards in double screw extruder (LD40, diameter 52mm, parallel double-screw) main feeding hopper, Unined RM antiseptics are fed in side
Material mouth is added, and is granulated in 150-220 DEG C of temperature range, tie rod water cooling pelletizing, and 100 DEG C of recirculated hot air is dried 30 minutes, is made
Antibacterial matrices.Double screw extruder temperature is set：1 150 DEG C of area, 165 DEG C of 2nd area, 180 DEG C of 3rd area, 170 DEG C of 4th area, 205 DEG C of 5th area, 6
210 DEG C of area, 220 DEG C of 7th area, 205 DEG C of 8th area.
The preparation method of the Unined RM antiseptics is the same as embodiment 1.
The preparation method of the expanded graphite of the surface treatment is the same as embodiment 10.
The preparation method of the coupling agent is the same as embodiment 11.
By the antibacterial matrices of acquisition and common polythene section in mass ratio 20:80 ratios mix, and obtain compound, actual
Unined net content is 2.0%.Compound is fitted into injection machine, injecting machine material tube temperature is followed successively by：1 220 DEG C of area, 2nd area
220 DEG C, 3 215 DEG C of areas, 4 215 DEG C of areas, 5 210 DEG C of areas, 6 210 DEG C of areas, 7 200 DEG C of areas, 8 190 DEG C of areas, 9 180 DEG C of areas, mold temperature
30 DEG C, 4cm × 6cm × 0.1cm plaques are made on 350MT injection machines.
The obtained original antibacterial activity value test result of print：Escherichia coli 5.0, methicillin-resistant staphylococcus aureus
4.9, staphylococcus aureus 4.9, Candida albicans 4.9, Friedlander's bacillus 4.8；
Antibacterial activity test result after obtained long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths warm water immersion：Greatly
Enterobacteria 5.0, methicillin-resistant staphylococcus aureus 4.9, staphylococcus aureus 5.0, Candida albicans 4.9, pneumonia gram
The primary Salmonella 4.8 of thunder；
Obtained print oxygen index (OI) test result：35.8%.
Test case 1
The print obtained to embodiment 4-14 and comparative example 1-4 carries out anti-microbial property test.
Concrete outcome is shown in Table 1.
The original antibacterial activity value of the print of table 1
Embodiment 4-7 antibacterial activity is substantially better than comparative example 1-4, and embodiment 4-7 all shows that antibacterial activity value is all super
0.5 is crossed, illustrates that the present invention has the bacteriostasis of practicality.
Embodiment 10 is better than the (polyethylene of embodiment 7 using the expanded graphite of surface treatment as lubricant, antibacterial activity
Wax), embodiment 8 (butyl stearate), embodiment 9 (expanded graphite), after surface treatment expanded graphite greasy property improve,
Scattered more uniform, the antibacterial activity of the print of raising of antiseptic in the polymer.
Embodiment 11 is better than (the gamma-aminopropyl-triethoxy silicon of embodiment 10 using the coupling agent prepared, its antibacterial activity
Alkane), embodiment 12 (γ-(methacryloxypropyl) propyl trimethoxy silicane), embodiment 13 (VTES).
Test case 2
The print obtained to embodiment 4-14 and comparative example 1-4 carries out warm water immersion test, anti-after test warm water immersion
Bacterium activity value.
Concrete outcome is shown in Table 2.
Antibacterial activity value after the immersion of the warm water of table 2
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 of comparative example are greatly reduced the degree that can not be used.
Test case 3
The print oxygen index (OI) that embodiment 7-14 is obtained is measured, concrete outcome is shown in Table 3.
The oxygen index (OI) test result of table 3
| Oxygen index (OI), % | |
| Embodiment 7 | 28.3 |
| Embodiment 8 | 28.1 |
| Embodiment 9 | 30.6 |
| Embodiment 10 | 31.9 |
| Embodiment 11 | 33.2 |
| Embodiment 12 | 31.1 |
| Embodiment 13 | 31.6 |
| Embodiment 14 | 31.3 |
Test case 4
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 it is other using polyolefin or
In the Application of composite of polyolefine material.By the master batch that embodiment 2 obtains by 5% weight than adding HDPE (MI=20g/10min),
Then after carrying out bicomponent spin with PET 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 antibacterial test according to standard GB/T20944.3-2008.Testing strain is：ETEC
It is ATCC25922 (Escherichia coli), staphylococcus aureus ATCC25923 (Staphyl DEG C DEG C of cus aureus), white
Color candida albicans ATCC10231 (Candida albicans), Shigella ATCC12022 (Shigellosis), salmonella
ATCC8014 (Salmonella), pseudomonas aeruginosa ATCC27853 (Pseudomonas aeruginosa), hemolytic hammer
Bacterium (Hemolytic strept DEG C DEG C us).
Concrete outcome is shown in Table 4.
The bacteriostasis rate test result of the non-woven fabrics of table 4
From table 4, it can be seen that non-woven fabrics is above 70% to the bacteriostasis rate of the strain of test, meet antibacterial requirement.
Claims (10)
- A kind of 1. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths, it is characterised in that long acting antibiotic polyethylene ES hot blast antibacterials The raw material of non-woven fabrics includes the antibacterial matrices that percentage by weight is 2-5%.
- 2. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 1, it is characterised in that the antibacterial matrices bag Include the raw material of following weight percentage：Unined RM antiseptics 5-20%, lubricant 0.1-1%, coupling agent 0.1-0.5%, it is remaining Measure as high-density polyethylene plastics resin；The Unined RM antiseptics include the raw material of following weight parts：Dispersant 0.2-8 parts, acrylic acid 0.56-20.5 parts, Phenols 10-15 parts, phellodendron extract 3-5 parts, rue leaf extract 6-10 parts, methyl resveratrol 2-4 parts, glycitin 3-5 Part, 2,4,5,6- tetrachloro phthalonitrile 3-5 parts；The phenols is the one or more combination thing in isopropyl methyl phenol, triclosan, antiphen, clorofene, chloreresol；The melt flow rate of the high-density polyethylene plastics resin is MI=20g/10min, 190 DEG C/21.6kg of experimental condition；The lubricant is one kind in expanded graphite, Tissuemat E, butyl stearate, and the expanded graphite is surface treatment Expanded graphite.
- 3. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 2, it is characterised in that the lubricant is table The expanded graphite and/or butyl stearate of face processing.
- 4. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 2, it is characterised in that the coupling agent is under The method of stating is prepared：(1) by gamma-aminopropyl-triethoxy-silane and cinnamic acid in molar ratio (2-5)：1 mixing, obtains mixture, adds mixed The ethanol of 4-6 times of compound quality, at 20-30 DEG C with 100-200 revs/min of stirring 10-20 minute, obtain mixed solution A；(2) mass fraction is added in mixed solution A and is 98% concentrated sulfuric acid, then be warming up to 60-80 DEG C, stirred with 100-200 revs/min 8-12 hours are mixed, obtain solution B, the wherein mass ratio of mixed solution A and the concentrated sulfuric acid is 1:(0.01-0.05)；(3) mixed solution B has been concentrated under reduced pressure into crystal precipitation under the conditions of pressure is 60Pa, temperature is 40-60 DEG C, 10-20 DEG C of placement 1-3 hour, with 300 mesh filter-cloth filterings, solid is dried to constant weight in 40-60 DEG C of vacuum drying chamber, obtains idol Join agent.
- 5. the long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as described in Claims 2 or 3, it is characterised in that at the surface The expanded graphite of reason is prepared by following methods：(1) by the concentrated sulfuric acid and mass fraction that mass fraction is 98% be 30% hydrogen peroxide by volume (6-10):1 is mixed Close, obtain mixed liquor, crystalline flake graphite and mixed liquor are pressed into solid-to-liquid ratio 1g：(3-6) mL mix, 25-35 DEG C with 100-200 turn/ Divide stirring 60-80 minutes, with 300 mesh filter-cloth filterings, it is 5-7 that solid, which is washed with deionized to water outlet pH, and squama is added in solid The acetic acid of 2-4 times of piece graphite quality, at 25-35 DEG C with 100-200 revs/min of stirring 2-3 hour, with 300 mesh filter-cloth filterings, to solid It is 5-7 that body, which is washed with deionized to water outlet pH, and solid dries 2-3 hours in 60-70 DEG C of drying box, obtains intercalated graphite；(2) intercalated graphite is incubated the 20-40 seconds in 700-900 DEG C of Muffle furnace, takes out, obtain expanded graphite；(3) expanded graphite and mass fraction are pressed into solid-to-liquid ratio 1g for 5-10% sodium dodecyl benzene sulfonate aqueous solution：(5-10) ML is mixed, and at 40-60 DEG C with 200-300 revs/min of stirring 60-80 minute, using 300 mesh filter-cloth filterings, solid is being dried in vacuo With 60-70 DEG C of dry expanded graphite 2-4 hours, being surface-treated in case.
- 6. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 2, it is characterised in that the phellodendron extract It is prepared by following methods：(1) water extraction：Golden cypress is cleaned, in 40-50 DEG C of dry 3-5 hour, obtains drying golden cypress, adds and dry golden cypress weight 6-10 Distilled water again, then 40-60 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, filtrate A is obtained, is added in filter residue dry The distilled water of dry 4-6 times of golden cypress weight, then 30-40 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, liquor B is obtained, The distilled water for drying 4-6 times of golden cypress weight is added in filter residue, then 30-40 minutes are incubated at 95-98 DEG C, using 300 mesh filter cloth mistakes Filter, liquor C is obtained, merging filtrate A, liquor B, liquor C, it is 1.3-1.35's (50 DEG C) that relative density is concentrated at 40-60 DEG C Concentrate；(2) volume fraction that 5 times of concentrate weight is added in concentrate is 95% ethanol water, is stirred with 100-200 revs/min Mix 10-20 minutes, stand 6-14 hours, with 3000-5000 revs/min centrifugation 5-10 minutes, by supernatant pressure be 60Pa, temperature Spend for the concentrate that recovery ethanol to relative density is 1.3-1.35 (50 DEG C) that is concentrated under reduced pressure under the conditions of 40-60 DEG C, using 200 mesh Filter-cloth filtering, filtrate are dried in vacuo 10-20 hours at 40-60 DEG C, vacuum 60Pa, obtain phellodendron extract.
- 7. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 2, it is characterised in that the rue leaf extraction Thing is prepared by following methods：(1) rue leaf is cleaned, in 40-50 DEG C of dry 3-5 hour, obtains drying rue leaf, add and dry rue leaf weight 6- 10 times of distilled water, then 40-60 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, filtrate A is obtained, is added in filter residue The distilled water of 4-6 times of rue leaf weight is dried, then 30-40 minutes are incubated at 95-98 DEG C, using 300 mesh filter-cloth filterings, is filtered Liquid B, adds the distilled water for drying 4-6 times of rue leaf weight in filter residue, then in 95-98 DEG C of insulation 30-40 minute, using 300 mesh Filter-cloth filtering, liquor C is obtained, merging filtrate A, liquor B, liquor C, it is 1.5-1.65 (50 that relative density is concentrated at 40-60 DEG C DEG C) concentrate；(2) volume fraction that 4 times of concentrate weight is added in concentrate is 95% ethanol water, is stirred with 100-200 revs/min Mix 10-20 minutes, stand 6-14 hours, with 3000-5000 revs/min centrifugation 5-10 minutes, by supernatant pressure be 60Pa, temperature Spend for the concentrate that recovery ethanol to relative density is 1.5-1.65 (50 DEG C) that is concentrated under reduced pressure under the conditions of 40-60 DEG C, using 200 mesh Filter-cloth filtering, filtrate are dried in vacuo 10-20 hours at 40-60 DEG C, vacuum 60Pa, obtain rue leaf extract.
- 8. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 2, it is characterised in that the Unined RM Antiseptic is prepared by following methods：(1) by load weighted phenols, phellodendron extract, rue leaf extract, methyl resveratrol, glycitin, 2,4,5,6- Tetrachloro phthalonitrile, dispersant 20-30 DEG C mixing, after mixing under 90-95 DEG C, 500-550mm mercury column reduced pressures with 300-500 revs/min of stirring 40-60 hour, obtain powder；(2) powder that step (1) obtains is mixed with acrylic acid, in 90-95 DEG C, 500-550mm mercury column reduced pressures after mixing Under with 300-500 revs/min stirring 40-60 hours.
- 9. long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths as claimed in claim 2, it is characterised in that the antibacterial matrices by Following methods are prepared：High-density polyethylene plastics resin, lubricant, coupling agent are weighed by formula, is put into mixer, 200-500r/min, 25-50 DEG C of stirring 10-30min, stir 2-10min by rotational speed regulation to 600-800r/min, are then fed into In double screw extruder main feeding hopper, Unined RM antiseptics add in side spout, in 150-220 DEG C of melting extrusion, cold But, it is granulated, antibacterial matrices is made.
- 10. the preparation method of long acting antibiotic polyethylene ES hot blast antibacterial nonwoven cloths, its feature as described in claim any one of 1-9 Be, be included in the antibacterial matrices for adding that percentage by weight is 2-5% in non-woven fabrics raw material, prepare non-woven fabrics by existing process and .
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