CN104310795B - A kind of preparation method of substrate surface antimicrobial coating - Google Patents
A kind of preparation method of substrate surface antimicrobial coating Download PDFInfo
- Publication number
- CN104310795B CN104310795B CN201410513141.3A CN201410513141A CN104310795B CN 104310795 B CN104310795 B CN 104310795B CN 201410513141 A CN201410513141 A CN 201410513141A CN 104310795 B CN104310795 B CN 104310795B
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- China
- Prior art keywords
- base material
- substrate surface
- nafion
- antimicrobial coating
- preparation
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Abstract
The invention discloses a kind of method that substrate surface prepares Nafion bromo-furanone composite antibacterial coating, it is characterised in that said method comprising the steps of: (1) base material pretreatment；(2) Nafion bromo-furanone composite antibacterial coating is prepared at substrate surface.The method has that simple to operate, the suitability is strong, low cost and the advantage such as pollution-free, it it is a kind of biomembrane control method based on non-bactericidal mechanism, the problem overcoming the bacterial drug resistance enhancing that classical antibacterial agents causes, and mixed vaccine biomembrane and pure bacterium biomembrane are all had good antibacterial effect.
Description
Technical field
The present invention relates to a kind of method preparing Nafion-bromo-furanone composite antibacterial coating at substrate surface, belong to biomembrane control
Technical field processed.
Background technology
Biomembrane (biofilm) is by being attached to inertia or the microorganism on active entities surface and being wrapped in the hydrability of microorganism
The structural microbiologic population that substrate is formed is constituted.Antibacterial in biomembrane is by the extracellular polymeric (EPS) of himself secretion
By Cell binding together, complicated microbial cell group is formed.The formation of harmful organism film can cause a lot of problem.Doctor
Field, it is to be caused by biomembrane that the human body antibacterial of about 80% infects.At environmental area, membrane bioreactor surface biological film
Formation can increase transmembrane pressure, causes effluent quality to deteriorate, and seriously hinders the extensive application of membrane technology.Biofilm contamination there is also
In water supply and sewerage pipeline system.There are some researches show, the drinking water treatment systems of 95% is all polluted by bacterial biof iotalm, to drink
Water safety brings potential risk.Therefore, the formation of effective suppression harmful organism film be a lot of field face severe challenge it
One.
In the past for using antibacterial to kill antibacterial biomembranous control, as used the antibacterial such as antibiotic, silver and chlorine more.Though
So antibacterial can suppress biomembranous growth to a certain extent, but there is also a lot of problem simultaneously.Due to planktonic bacteria
After forming biomembrane, phenotype changes so that biomembrane is 1000 times of planktonic bacteria to the Drug resistance of classical antibacterial agents, so
Traditional antibacterial is used to be difficult to the antibacterial within biomembrane is worked.Long-term excessively use antibiotic also results in the anti-of antibacterial
The property of medicine increases, and makes drug-resistant bacteria spread.Membranous system can be caused damage by some oxidized form antibacterial (such as chlorine, ozone etc.), and
And it is likely to form disinfection byproduct (DBP).Therefore, it is necessary to set up a kind of brand-new biomembrane control method.
Quorum sensing (quorum sensing, QS) is also referred to as self-induction, refers to that antibacterial regulates a kind of ring of self cell density
Border induction system, by the little molecule of diffusibility signal (being also called self-induction agent, autoinducer, AI) and Activator protein
Interact and express the gene relevant with cell colony density.These signaling molecules are diffused into environment from bacterial cell, when reaching
Transcribing of a series of target genes is regulated to just inducing during critical concentration (reaching a certain specific population density in other words),
Generation including the synthesis of enzyme, biomembranous formation, the biosynthesis of antibiotic and biosurfactant etc..Therefore, resistance
Signal communication between disconnected antibacterial is likely to become a kind of new method of suppression biofilm formation.Quorum sensing inhibitor (quorum
Sensing inhibitors, QSIs) it is a kind of material that can interfere with antibacterial QS system.Natural or the bromo furan of synthetic
Ketone (BFs) is to study most commonly used class QSI at present, and they can be competed with N-acyl-homoserine lactone (AHL)
Its intracellular specific receptors-LuxR family protein, thus block the QS system of antibacterial.Also there are some researches show that some bromo-furanones can
To disturb AI-2QS system, thus suppress biomembranous formation.
The method controlling substrate surface biological pollution includes surface modification and loads antibacterial/fungistatic coating.Number of patent application
200710016018.0 surfaces that by the way of chemical bonding, nano-Ag particles is fixed on production equipment, it is thus achieved that long-acting, tool
There is the nanometer antibacterium coating of slow release characteristic, it is achieved that to control biomembranous in beer equipment.Chuang etc. (2008) are by antibacterial
Agent (silver nitrate or cetrimonium bromide) has loaded to be formed in polyacrylic acid and polymine polyelectrolyte coating.Schmidt
Deng (2010), antibacterial gentamycin has been assembled into the polymerization electricity of degradable poly-amino ester, hyaluronic acid or polyacrylic acid formation
Solving in matter coating, along with the degraded of polymer, gentamycin is released, and restrained effectively staphylococcus aureus biological
The formation of film.Antibacterial paclitaxel is successfully loaded to be formed in hyaluronic acid and antibacterial sugar polymer electrolyte by Thierry etc. (2005)
Matter coating.But, these coating shortcomings being loaded with antibacterial are as the increase of bacterial drug resistance, its bacteriostasis antibiosis effect meeting
It is substantially reduced.In order to solve these problems, this patent proposes a kind of colony induction signaling molecule inhibitor of utilization, uses Nafion
Polymer is loaded prepares antibacterial/antimicrobial coating, suppresses biofilm formation by non-sterilization mode.Nafion is a kind of sulfonation four
Fluoride copolymers, is made up of the sulfonic acid group on a fluorocarbon skeleton and its side chain.The aquaporin model reason of Nafion
Opinion proposes its inside configuration and arranges a series of hydrophilic channel, each passage about 2.5nm, can transport small ion.At solution
Sulfonic acid group on middle Nafion side chain can hydrolysis H+So that its surface is electronegative.Owing to most antibacterial is electronegative,
So depositing electrostatic repulsion between Nafion and antibacterial, antibacterial can be hindered in the attachment on its surface.Utilize Nafion and bromo furan
Ketone of muttering coupling is prepared the method for antibacterial/antimicrobial coating and be there is not yet relevant report.
Summary of the invention
It is an object of the invention to propose the preparation method of a kind of substrate surface antimicrobial coating.The present invention by one bromo-furanone,
(Z-) in the bromo-5-of-4-(bromine ethylene)-2 (5H)-furanone (BBF) loads to the aquaporin of Nafion polymer, at substrate surface structure
Build a Nafion-BBF composite antibacterial coating.The machine of constructed Nafion-BBF composite antibacterial coating suppression biofilm formation
Reason is: hydrolysis H in the solution of the sulfonic acid group on Nafion side chain+Make coating surface electronegative, the electrostatic repulsion energy of generation
Enough hinder antibacterial in its surface adhesion；BBF is a kind of signaling molecule quencher, when it delays from the aquaporin of Nafion polymer
On The Drug Release out after, its intracellular receptor albumen can be competed with the signaling molecule of antibacterial, hinder the table with biofilm formation related gene
Reach, the QS system of interference antibacterial, thus suppress biomembranous formation.Bromo-furanone and Nafion coupling is utilized to prepare antibacterial
The method of coating, has that biomembrane inhibition is notable, simple to operate, the suitability strong, low cost and an advantage such as pollution-free.By
It is a kind of biomembrane control method based on non-bactericidal mechanism in this method, which overcomes the bacterial resistance that classical antibacterial agents causes
Property strengthen problem.The proposition of the method provides new thinking for biomembranous control, has important theory value and practice
Meaning, is expected to be used for solving the Biofilm contamination difficult problem in the field such as environment, medical science.
The present invention proposes a kind of method utilizing bromo-furanone and Nafion coupling to prepare antimicrobial coating at substrate surface, and it is special
Levy and be, said method comprising the steps of:
(1) base material pretreatment
Described base material is selected from glass baseplate (such as microscope slide, coverslip), metal base (such as copper sheet, titanium plate, steel disc) etc.
In one；
The pre-treatment step of glass baseplate includes: cleaning with cleaning agent, deionized water rinse, after methanol rinses, nitrogen is dried, so
Silanization treatment is carried out afterwards by aminopropyltriethoxywerene werene；
The pre-treatment step of metal base includes: surface finish, the most successively with distilled water, acetone and dehydrated alcohol ultrasonic cleaning,
Finally it is vacuum dried.
(2) composite antibacterial coating is prepared
The preparation of composite antibacterial coating uses layer by layer deposition method, by step i) or step ii) compound in substrate surface preparation
Antimicrobial coating:
I) 30min-12h during first pretreated base material is immersed in 0.1%-2%Nafion ethanol solution, empty after taking out base material
Air dry is dry, impregnated in 1-30mg/L BBF ethanol solution the most again, and after taking out after 30min-12h, air drying is standby；
Ii) pretreated base material is immersed in the mixed solution containing 0.1%-2%Nafion and 1-30mg/L BBF, and 30
Taking out after min-12h, air drying is standby.
Beneficial effect
(1) the Nafion-BBF method for preparing antibiotic coating that the present invention proposes, has base simple, easy to operate, applicable
The advantages such as material is extensive；
(2) the Nafion-BBF composite antibacterial coating that the present invention proposes all has good suppression to pure bacterium and mixed vaccine biomembrane
Effect, suppression ratio biomembranous to mixed vaccine in sewerage is 50-70%, to pure bacterium Pseudomonas aeruginosa, escherichia coli and withered
The grass biomembranous suppression ratio of bacillus cereus is 30-60%；
(3) antimicrobial component in the composite antibacterial coating that prepared by the present invention is Nafion and BBF, is different from based on bactericidal mechanism
Traditional antibacterial, such as antibiotic, silver and chlorine etc., which overcome biomembrane control method based on bactericidal mechanism may produce
Raw microorganism drug resistance problems.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite antibacterial coating of preparation in the embodiment of the present invention 1.
Fig. 2 is the atomic force microscope figure of the composite antibacterial coating of preparation in the embodiment of the present invention 3.
Fig. 3 is the composite antibacterial coating inhibition biomembranous to mixed vaccine of preparation in the embodiment of the present invention 3.
Fig. 4 is the composite antibacterial coating inhibition biomembranous to pure bacterium of preparation in the embodiment of the present invention 5.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but present disclosure is not
It is limited only to the following examples:
Embodiment 1
(1) first titanium plate carries out surface finish, the most successively by distilled water, acetone and dehydrated alcohol ultrasonic cleaning, last vacuum
It is dried；
(2) the titanium plate of pretreatment is immersed in the mixed solution containing 1%Nafion and 10mg/L BBF, takes out after 12h,
Air saves backup after drying；
(3) Fig. 1 is the scanning electron microscope (SEM) photograph of antimicrobial coating prepared by the present embodiment.The antimicrobial coating preparing the present embodiment resists
Bacterium performance test, takes from mixed vaccine bacteria suspension prepared by the activated sludge of sewage treatment plant and shows as experimental subject, result, raw
After thing Membrance cuiture one day, antimicrobial coating suppression ratio biomembranous to mixed vaccine is 61%.
Embodiment 2
(1) first titanium plate carries out surface finish, the most successively by distilled water, acetone and dehydrated alcohol ultrasonic cleaning, last vacuum
It is dried；
(2) the titanium plate of pretreatment is immersed in the mixed solution containing 0.5%Nafion and 10mg/L BBF, takes after 12h
Going out, air saves backup after drying；
(3) antimicrobial coating preparing the present embodiment carries out anti-microbial property experiment, takes from prepared by the activated sludge of sewage treatment plant
Mixed vaccine bacteria suspension shows as experimental subject, result, and after biomembrane is cultivated one day, antimicrobial coating presses down mixed vaccine is biomembranous
Rate processed is 49%.
Embodiment 3
(1) first microscope slide is dried with nitrogen after cleaning agent cleaning, deionized water rinse, methanol rinses, then uses aminopropyl
Triethoxysilane carries out silanization treatment；
(2) microscope slide of pretreatment is immersed in the mixed solution containing 1%Nafion and 10mg/L BBF, takes after 12h
Going out, air saves backup after drying；
(3) Fig. 2 is the atomic force microscope figure of antimicrobial coating prepared by the present embodiment.The antimicrobial coating preparing the present embodiment enters
Row anti-microbial property is tested, and takes from mixed vaccine bacteria suspension prepared by the activated sludge of sewage treatment plant as experimental subject, result such as figure
Shown in 3, after biomembrane cultivates 6h, antimicrobial coating suppression ratio biomembranous to mixed vaccine is 43%；When incubation time extends to
12-72h, antimicrobial coating still has significant biomembrane suppression ratio (28%-51%).
Embodiment 4
(1) first microscope slide is dried with nitrogen after cleaning agent cleaning, deionized water rinse, methanol rinses, then uses aminopropyl
Triethoxysilane carries out silanization treatment；
(2) microscope slide of pretreatment is immersed in the mixed solution containing 1%Nafion and 20mg/L BBF, takes after 12h
Going out, air saves backup after drying；
(3) antimicrobial coating preparing the present embodiment carries out anti-microbial property experiment, takes from prepared by the activated sludge of sewage treatment plant
Mixed vaccine bacteria suspension shows as experimental subject, result, and after biomembrane is cultivated one day, antimicrobial coating presses down mixed vaccine is biomembranous
Rate processed is 56%.
Embodiment 5
(1) first microscope slide is dried with nitrogen after cleaning agent cleaning, deionized water rinse, methanol rinses, then uses aminopropyl
Triethoxysilane carries out silanization treatment；
(2) first the microscope slide of pretreatment is immersed in 6h in 1%Nafion solution, takes out microscope slide air and soak the most again
Stain, in 10mg/LBBF solution, is taken out after 6h, and air saves backup after drying；
(3) antimicrobial coating preparing the present embodiment carries out Anti-microbial Performance Tests, selects Pseudomonas aeruginosa, escherichia coli and withered
Grass bacillus cereus be experimental subject, result as shown in Figure 4, biomembrane cultivate two days later, antimicrobial coating to Pseudomonas aeruginosa,
Escherichia coli and the biomembranous suppression ratio of bacillus subtilis are respectively 23%, 37% and 48%.
Claims (4)
1. the preparation method of a substrate surface antimicrobial coating, it is characterised in that the method comprises the following steps:
(1) base material pretreatment；
(2) by step i) or step ii) prepare composite antibacterial coating at substrate surface:
I) 30min-12h during first pretreated base material is immersed in 0.1%-2% Nafion ethanol solution, empty after taking out base material
Air dry is dry, impregnated in 1-30mg/L BBF ethanol solution the most again, and after taking out after 30min-12h, air drying is standby；
Ii) pretreated base material is immersed in the mixed solution containing 0.1%-2%Nafion and 1-30mg/L BBF, and 30
Taking out after min-12h, air drying is standby.
The preparation method of a kind of substrate surface antimicrobial coating the most according to claim 1, it is characterised in that described in (1)
Base material be the one in glass baseplate and metal base.
The preparation method of a kind of substrate surface antimicrobial coating the most according to claim 1, it is characterised in that described in (1)
Base material pretreatment, when base material is glass baseplate, first with nitrogen after cleaning agent cleaning, deionized water rinse, methanol rinses
It is dried, then carries out silanization treatment by aminopropyltriethoxywerene werene.
The preparation method of a kind of substrate surface antimicrobial coating the most according to claim 1, it is characterised in that described in (1)
Base material pretreatment, when base material is metal base, first carry out surface finish, the most successively with distilled water, acetone and anhydrous
EtOH Sonicate cleans, and is finally vacuum dried.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021212153A3 (en) * | 2020-04-17 | 2021-11-25 | Kraton Polymers Llc | Antimicrobial spray composition |
| WO2021212147A3 (en) * | 2020-04-17 | 2021-12-02 | Kraton Polymers Llc | Bio-secure protective equipment and methods for making |
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| CN105771687B (en) * | 2016-03-29 | 2019-09-03 | 天津工业大学 | A kind of preparation method of antibacterial PVC ultrafiltration membrane |
| CN105859154A (en) * | 2016-04-07 | 2016-08-17 | 厦门大学 | Preparation method of sulfonyl-modified anti-biological pollution coating |
| EP3488699A4 (en) * | 2016-07-21 | 2019-05-29 | FUJIFILM Corporation | Antibacterial composition, antibacterial film, substrate with antibacterial film, method for manufacturing antibacterial film, and method for manufacturing substrate with antibacterial film |
| CN111299267B (en) * | 2020-02-12 | 2021-10-22 | 上海交通大学 | Water supply pipe network biofilm control method based on group induction effect and application thereof |
| WO2021212155A1 (en) * | 2020-04-17 | 2021-10-21 | Kraton Polymers Llc | Antimicrobial paint composition |
| CN113413764A (en) * | 2021-06-24 | 2021-09-21 | 南京财经大学 | Modified membrane module, preparation method thereof and application thereof in filtration |
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| US6387379B1 (en) * | 1987-04-10 | 2002-05-14 | University Of Florida | Biofunctional surface modified ocular implants, surgical instruments, medical devices, prostheses, contact lenses and the like |
| CN1557756A (en) * | 2003-02-20 | 2004-12-29 | ��ķ�ж���˾ | Antimicrobial glass and glass-like products and method of preparing same |
| CN103509396A (en) * | 2013-09-15 | 2014-01-15 | 浙江大学 | Preparation method of novel hydrophobic anti-microbial coating |
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| US20050129742A1 (en) * | 2003-12-16 | 2005-06-16 | Eastman Kodak Company | Antimicrobial article with diffusion control layer |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6387379B1 (en) * | 1987-04-10 | 2002-05-14 | University Of Florida | Biofunctional surface modified ocular implants, surgical instruments, medical devices, prostheses, contact lenses and the like |
| CN1557756A (en) * | 2003-02-20 | 2004-12-29 | ��ķ�ж���˾ | Antimicrobial glass and glass-like products and method of preparing same |
| CN103509396A (en) * | 2013-09-15 | 2014-01-15 | 浙江大学 | Preparation method of novel hydrophobic anti-microbial coating |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021212153A3 (en) * | 2020-04-17 | 2021-11-25 | Kraton Polymers Llc | Antimicrobial spray composition |
| WO2021212147A3 (en) * | 2020-04-17 | 2021-12-02 | Kraton Polymers Llc | Bio-secure protective equipment and methods for making |
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