CN109651942A - A kind of preparation method of super hydrophilic antimicrobial coating - Google Patents
A kind of preparation method of super hydrophilic antimicrobial coating Download PDFInfo
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- CN109651942A CN109651942A CN201811533450.1A CN201811533450A CN109651942A CN 109651942 A CN109651942 A CN 109651942A CN 201811533450 A CN201811533450 A CN 201811533450A CN 109651942 A CN109651942 A CN 109651942A
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- antimicrobial coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
- C09D171/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The present invention discloses a kind of preparation method of super hydrophilic antimicrobial coating, comprising the following steps: substrate material cleaning, gas ions pretreatment, the coating of polyethylene glycol component and polymerization crosslinking.Super hydrophilic antimicrobial coating of the invention, ingredient are all biocompatible materials, have the function of anti-bacterial attachment, and stability is preferable, and broad-spectrum antibacterial property is good, have preferable inhibitory effect to gram-positive bacteria, negative bacterium, fungi；The method that the present invention prepares super hydrophilic antimicrobial coating carries out in aqueous phase system, without using organic solvent, green non-pollution；Super hydrophilic antimicrobial coating prepared by the present invention and base material are to be not easy to be destroyed or influenced by external environment, to realize non-medication antibacterial by covalent bond and Hydrogenbond.
Description
Technical field
The present invention relates to anti-biotic material technical fields, and in particular to a kind of preparation method of super hydrophilic antimicrobial coating.
Background technique
In the natural environment, the microorganisms such as bacterium usually aggregation growth on the surface of the material, and interconnect and generate extracellularly
Polymer, to form bacterial biof iotalm.When bacterial adhesion is on medical device materials surface, and then it is grown to bacterium living beings
Film then easily causes human infection relevant to instrument, causes various health problems.The study found that bacterium is easier to be attached to
On the material surface of albumin layer absorption, therefore anti-protein absorption surface should also inhibit bacterial adsorption.Polyethylene glycol is a kind of
Using-CH2-CH2-O- as constitutional repeating unit, and the macromolecule that both ends are blocked with hydroxyl group, there is excellent anti-protein adsorption
Ability.Researcher has found in the substrate that polyethylene glycol preparation on probation can be adsorbed with antibacterium, polyethylene glycol very flexibly and
Very large space resistance is showed, this will hinder bacterial adhesion to material surface.
Currently, using the method for the compound-modified material surface of polyethylene glycols be mostly physics dip-coating, chemical graft, etc.
Gas ions polymerization crosslinking.The polyethylene glycol coating stability obtained on the surface of the material by physics dip-coating is poor, is easy to peel off, cannot
Meet actual clinical demand；And although coating that chemical graft obtains is more stable, but its process is needed using organic solvent,
And process is more complicated, higher cost, biocompatibility is still to be tested.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide one kind can be by low temperature plasma at
To there is the complicated macromolecule polyalcohol of-CH2-CH2-O- structure fragment to be bonded in super parent obtained on substrate for reason and chemistry coating
The preparation method of water antimicrobial coating.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of preparation method of super hydrophilic antimicrobial coating,
It is characterized in that, comprising the following steps:
S1, substrate material cleaning: substrate is cleaned, and to remove surface impurity, greasy dirt, then uses distilled water flushing, then dry
It does spare；
S2, gas ions pretreatment: using plasma carries out any one in surface active and functionalization or two kinds of groups to substrate
Conjunction is handled；
The coating of S3, polyethylene glycol component: 5%~25% solution that polyethylene glycol component compound is made into, for coating warp
The processed substrate of step 2 is crossed, is bonded polyethylene glycol component with the substrate surface of functionalization, after 0.25~1h, uses distilled water
It rinses, then is dried for standby, the polyethylene glycol component compound is one or more groups containing-CH2-CH2-O- structure fragment
It closes, the average molecular weight of the polyethylene glycol is in 200-7000；
S4, polymerization crosslinking: corona treatment is carried out to the substrate that step 3 is handled well using plasma, makes the poly- second of coating
Diol component compound is cross-linked to each other, and forms a kind of complicated macromolecule polyalcohol with-CH2-CH2-O- structure fragment
The super hydrophilic antimicrobial coating is made.
Further, the surface activation process in the step 2 are as follows: the substrate handled by step 1 is put into plasma
In fluid chamber, the plasma chamber is vacuumized, is passed through non-polymerization gas, opens the plasma chamber electrode electricity
Source is discharged, and carries out surface active to the substrate；Vacuum degree is protected in plasma chamber room in the surface activation process
Hold between 20Pa-100Pa, temperature be maintained at 45 DEG C hereinafter, the flow of the non-polymerization gas in 20sccm-300sccm
Between, the discharge time is 2min-20min.
Further, the functionalization in the step 2 are as follows: by reactant gas for two kinds of gases and with volume ratio 1:
50~1:1 is passed through in the plasma chamber room, is opened the plasma chamber electrode power supply and is discharged, and reactivity is generated
Polymerization reaction, generation polymer etc. occur in the plasma chamber room for gaseous plasma, the reactive plasma
Gas ions, the polymer is plasma-deposited to form super-hydrophilic coating presoma in the substrate surface；At the functionalization
Vacuum degree is maintained between 20Pa-100Pa in plasma chamber room in reason, and temperature is maintained at 45 DEG C hereinafter, the reactivity
For the flow of gas between 50sccm-450sccm, the discharge time is 3min-30min.
Further, the polymerization crosslinking processing in the step 3 are as follows: the substrate handled by step 3 is put into plasma
In fluid chamber, the plasma chamber is vacuumized, is passed through non-polymerization gas, opens the plasma chamber electrode electricity
Source is discharged, and the surface of the substrate is crosslinked；Vacuum degree is kept in plasma chamber room in the cross-linking step
Between 20Pa-100Pa, temperature be maintained at 45 DEG C hereinafter, the non-polymerization gas flow 50sccm-300sccm it
Between, the discharge time is 10s-2min.
Further, the discharge frequency of the plasma chamber electrode power supply is radio frequency 13.56MHZ, described in etc.
The discharge mode of plasma chamber electrode supply is continuous radio frequency discharge, and playing continuous radio frequency discharge power is 10W-1000W.
Further, the non-polymerization gas is O2、N2, one of Ar, Ne, He or multiple combinations.
Further, one of gas in the reactant gas is the gas that can generate oxygen radical, including
Vapor, O2、CO2、N2、NH3, one of Ar, He or multiple combinations；Another gas is short chain of the carbon atom number less than 6
Hydrocarbon, including CH4、C2H6、C2H4、C2H2、C3H8、C3H6、C4H10、C4H8、C5H12、C5H10One of or multiple combinations.
Further, the material of the substrate includes following at least one materials: polypropylene, high density polyethylene (HDPE), propylene
Nitrile-butadiene-styrene copolymer, polyethylene terephthalate, polymethyl methacrylate, polyvinyl chloride, polytetrafluoro
Ethylene, polyamide, polyurethane, silicon rubber, latex, silicon wafer, sheet glass, stainless steel, nickel alloy, titanium alloy.
Further, the substrate be the fiber made of substrate material, silk thread, woven cloths, non-woven fabrics, film, foam,
Thin slice, conduit or bracket.
After adopting the above structure, the invention has the following beneficial effects:
Super hydrophilic antimicrobial coating of the invention, ingredient are all biocompatible materials, have the function of anti-bacterial attachment, are stablized
Property is preferable, and broad-spectrum antibacterial property is good, has preferable inhibitory effect to gram-positive bacteria, negative bacterium, fungi；Present invention preparation is super
The method of hydrophilic antimicrobial coatings carries out in aqueous phase system, without using organic solvent, green non-pollution；It is prepared by the present invention
Super hydrophilic antimicrobial coating and base material be not easy to be destroyed or influenced by external environment by covalent bond and Hydrogenbond, thus
Realize non-medication antibacterial.
Detailed description of the invention
Fig. 1 is the effect picture in embodiment 1；
Fig. 2 is the effect picture in embodiment 2；
Fig. 3 is that control group slide is used for the obtained microscope photo of anti-bacterial attachment effect test in embodiment 3；
Fig. 4 is that embodiment 3 is super hydrophilic antimicrobial coating slide for the obtained microscope photo of anti-bacterial attachment effect test；
Fig. 5 is that the viable plate of control group polyurethane catheter in embodiment 4 counts photo；
Fig. 6 is that the viable plate of the super hydrophilic antimicrobial coating polyurethane catheter of 4 floating coat group of embodiment counts photo.
Specific embodiment
The present invention is further illustrated for following example.
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are only to explain the present invention, not
For limiting the present invention.
Embodiment 1
Contact angle test: slide, super hydrophilic antimicrobial coating slide before blank slide, dip-coating are connect respectively using contact angle instrument
The test of feeler, contact angle test carry out on the contact angle instrument of upper marine morning production, and inflow is 1.5 μ L.Test result is shown in
Fig. 1:
The initial contact angle a of glass slide, contact angle b before dip-coating, contact angle c photo after the completion of coating.
Embodiment 2
Contact angle test: blank conduit, dip-coating dummy pipe, super hydrophilic antimicrobial coating conduit are connect respectively using contact angle instrument
The test of feeler, contact angle test carry out on the contact angle instrument of upper marine morning production, and inflow is 1.5 μ L.Test result is shown in
Fig. 2:
The initial contact angle a of conduit, contact angle b before dip-coating, contact angle c photo after the completion of coating.
Integrated embodiment 1 and embodiment 2, super hydrophilic antimicrobial coating of the invention have good hydrophily, meet and use
Condition.
Embodiment 3
The anti-bacterial attachment effect test of the super hydrophilic antimicrobial coating of the present invention, concrete operations are as follows:
(1) prepare control group glass slide, with acetone, ethyl alcohol, water difference 10 min of ultrasound, then resist itself and the super hydrophilic of preparation
Bacterium coated glass slides sterilize under high steam, and after being cooled to room temperature, the big of 0.5 mL is added dropwise simultaneously in two groups of slide surfaces
Enterobacteria bacteria suspension (2 × 105cfu/mL of concentration), slide is put into the Bacteria Culture that disposable sterilized plate is placed in 35 ± 2 DEG C
In case.
(2) after cultivating 24 hours, the slide in plate is taken out, draws the aseptic water washing slide of 1mL every time with liquid-transfering gun
Surface repeats to rinse 5-6 times, then sucks the remaining water of surface of glass slide from slide surrounding with blotting paper.
(3) the crystal violet aqueous solution for preparing 1wt% dyes bacterium, and the knot of 0.3 mL is added dropwise in every surface of glass slide
Crystalviolet dyeing liquor makes dyeing liquor tile on slide as far as possible and covers microbionation region, covers plate at room temperature
Dye 30 min.
(4) it after dyeing, draws the dyeing liquor of the aseptic water washing surface of glass slide of 1mL every time with liquid-transfering gun, repeats to rush
It washes about 10 times, until slide is bright, without obvious bulk bluish violet dyeing liquor lacing film.It is residual that surface of glass slide finally is blotted with blotting paper again
The water stayed observes bacterial adhesion situation with optical microscopy.
Referring to Fig. 3-4, well-known to those skilled in the art, crystal violet can mutually be tied with the coating protein of bacterial secretory
It closes.Royal purple color dot on super hydrophilic composite antibacterial coating slide manufactured in the present embodiment it can be seen from Fig. 3 and Fig. 4 comparison is remote
Far fewer than control group, the effect of anti-bacterial attachment is prominent.
Embodiment 4
The antibacterial effect test of the super hydrophilic antimicrobial coating of the present invention, concrete operations are as follows:
(1) under aseptic technique, with the bacteria suspension for the Escherichia coli that normal saline concentration is 8 ~ 9 × 103 cfu/mL.
(2) prepare to have sterilized to parse the polyurethane catheter control group finished and coating group each 3, three sections are cut from every
As sample, each sample is respectively put into 15mL centrifuge tube, so 7cm by coating group sample totally 9 and 3 control group samples
It is separately added into the Escherichia coli bacteria suspension of 6mL step (1) preparation afterwards, the sample for being inoculated with Escherichia coli is then placed in 33 DEG C of perseverances
It is cultivated 17-19 hours in warm incubator.
(3) each sample after cultivating is gone out with sterile tweezer respectively, is put into 50ml centrifuge tube, uses the sterile life of 30ml every time
Reason salt water turns upside down 10 rinses, each sample rinse 3 times.The 15ml an of physiological saline containing 10ml is put into after rinse respectively
In centrifuge tube, 10 min of ultrasound in supersonic cleaning machine are placed on, 1ml ultrasonic cleaning liquid is then respectively taken to carry out the counting of viable bacteria a kind of rhyme scheme in Chinese operas serving as the prelude to a complete score for voices.
Referring to figs. 5 and 6, control group covers with bacterium, and what the bacterium of coating group can count comes out, and illustrates that control group has greatly
Bacterial adhesion is measured on conduit, and coating group have it is a small amount of or without bacterial adhesion on conduit, being computed antibiotic rate up to 90%
More than.
The above is only used to illustrate the technical scheme of the present invention and not to limit it, and those of ordinary skill in the art are to this hair
The other modifications or equivalent replacement that bright technical solution is made, as long as it does not depart from the spirit and scope of the technical scheme of the present invention,
It is intended to be within the scope of the claims of the invention.
Claims (9)
1. a kind of preparation method of super hydrophilic antimicrobial coating, which comprises the following steps:
S1, substrate material cleaning: substrate is cleaned, and to remove surface impurity, greasy dirt, then uses distilled water flushing, then dry
It does spare；
S2, gas ions pretreatment: using plasma carries out any one in surface active and functionalization or two kinds of groups to substrate
Conjunction is handled；
The coating of S3, polyethylene glycol component: 5%~25% solution that polyethylene glycol component compound is made into, for coating warp
The processed substrate of step 2 is crossed, is bonded polyethylene glycol component with the substrate surface of functionalization, after 0.25~1h, uses distilled water
It rinses, then is dried for standby, the polyethylene glycol component compound is one or more groups containing-CH2-CH2-O- structure fragment
It closes, the average molecular weight of the polyethylene glycol is in 200-7000；
S4, polymerization crosslinking: corona treatment is carried out to the substrate that step 3 is handled well using plasma, makes the poly- second of coating
Diol component compound is cross-linked to each other, and forms a kind of complicated macromolecule polyalcohol with-CH2-CH2-O- structure fragment
The super hydrophilic antimicrobial coating is made.
2. a kind of preparation method of super hydrophilic antimicrobial coating according to claim 1, it is characterised in that: in the step 2
Surface activation process are as follows: the substrate handled by step 1 is put into plasma chamber room, the plasma chamber is taken out
Vacuum is passed through non-polymerization gas, opens the plasma chamber electrode power supply and discharges, and carries out surface to the substrate
Activation；Vacuum degree is maintained between 20Pa-100Pa in plasma chamber room in the surface activation process, and temperature is maintained at
45 DEG C hereinafter, the flow of the non-polymerization gas between 20sccm-300sccm, the discharge time be 2min-20min.
3. a kind of preparation method of super hydrophilic antimicrobial coating according to claim 1, it is characterised in that: in the step 2
Functionalization are as follows: by reactant gas be two kinds of gases and the plasma chamber to be passed through with volume ratio 1:50~1:1
It is interior, open the plasma chamber electrode power supply and discharge, generate reactant gas plasma, the reactivity it is equal from
Polymerization reaction occurs in the plasma chamber room, generates polymer plasma for daughter, and the polymer plasma is heavy
Product forms super-hydrophilic coating presoma in the substrate surface；Vacuum degree is protected in plasma chamber room in the functionalization
Hold between 20Pa-100Pa, temperature be maintained at 45 DEG C hereinafter, the reactant gas flow 50sccm-450sccm it
Between, the discharge time is 3min-30min.
4. a kind of preparation method of super hydrophilic antimicrobial coating according to claim 1, it is characterised in that: in the step 3
Polymerization crosslinking processing are as follows: the substrate handled by step 3 is put into plasma chamber room, the plasma chamber is taken out
Vacuum is passed through non-polymerization gas, opens the plasma chamber electrode power supply and discharges, make the surface of the substrate into
Row crosslinking；Vacuum degree is maintained between 20Pa-100Pa in plasma chamber room in the cross-linking step, and temperature is maintained at 45
DEG C hereinafter, the flow of the non-polymerization gas between 50sccm-300sccm, the discharge time be 10s-2min.
5. according to preparation method described in claim 2-4 any one, it is characterised in that: the plasma chamber electrode electricity
The discharge frequency in source be radio frequency 13.56MHZ, described in plasma chamber electrode power supply discharge mode be continuous radio frequency put
Electricity, playing continuous radio frequency discharge power is 10W-1000W.
6. according to preparation method described in claim 2-4 any one, it is characterised in that: the non-polymerization gas is O2、
N2, one of Ar, Ne, He or multiple combinations.
7. a kind of preparation method of super hydrophilic antimicrobial coating according to claim 3, it is characterised in that: the reactivity gas
One of gas in body is the gas that can generate oxygen radical, including vapor, O2、CO2、N2、NH3, in Ar, He
One or more combinations；Another gas is short hydrocarbon of the carbon atom number less than 6, including CH4、C2H6、C2H4、C2H2、C3H8、
C3H6、C4H10、C4H8、C5H12、C5H10One of or multiple combinations.
8. a kind of preparation method of super hydrophilic antimicrobial coating according to claim 1, it is characterised in that: the material of the substrate
Material includes following at least one materials: polypropylene, acrylonitrile-butadiene-styrene copolymer, gathers to benzene high density polyethylene (HDPE)
Naphthalate, polymethyl methacrylate, polyvinyl chloride, polytetrafluoroethylene (PTFE), polyamide, polyurethane, silicon rubber, cream
Glue, silicon wafer, sheet glass, stainless steel, nickel alloy, titanium alloy.
9. a kind of preparation method of super hydrophilic antimicrobial coating according to claim 1 or 8, it is characterised in that: the substrate
It is the fiber made of substrate material, silk thread, woven cloths, non-woven fabrics, film, foam, thin slice, conduit or bracket.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110144569A (en) * | 2019-07-03 | 2019-08-20 | 东莞市和域战士纳米科技有限公司 | The preparation method of long-acting hydrophilic film |
| CN112239953A (en) * | 2020-09-17 | 2021-01-19 | 江苏盛纳凯尔医用科技有限公司 | Non-woven fabric surface treatment finishing agent composition and preparation method and application thereof |
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Application publication date: 20190419 |