CN104830124B - A kind of preparation method of stripe anti-tartar coating - Google Patents
A kind of preparation method of stripe anti-tartar coating Download PDFInfo
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Abstract
A kind of preparation method of stripe anti-tartar coating, the method combined using mask and light polymerization technique are prepared for a kind of coating material with antibiont dirt function of stripe.The antibiont dirt coating surface structure is polymer and the alternate stripe structure of base material, and pattern replaces for convex-concave, width is consistent, and range of coat thicknesses is between 100 300nm.It is (methyl) acrylate with zwitterion functional group or (methyl) acrylamide monomers that the monomer used by its floating coat is characterized by the monomer of antibiont dirt function, or polyethylene glycol (methyl) acrylate, or the monomer of fluorine replacement (methyl) acrylate structural.Stripe coating prepared by the present invention can keep intrinsic anti-fouling performance, and further lift antifouling capability.
Description
Technical field
The invention belongs to chemical field, is related to chemical coating, particularly a kind of surface has streaky antibiont dirt coating.
Background technology
Biofouling is also called biofouling, is often as material under water environment, microorganism precipitation occurs on its surface
Dirt is accumulated and is formed, common biofouling has albumen, bacterium, diatom, green alga, barnacle etc..The field affected by biofouling
Relate generally to two kinds：On the one hand it is marine field, including water process, submerged structure, hull etc., biofouling often causes excessively
Energy consumption, increase extra cost.On the other hand it is medical domain, such as medicine equipment infection etc..The research of antibiont dirt material
Widely paid close attention to.ZPT, pyrrole sulphur copper from the commercial product tributyl tin coating of last century the fifties to last decade
Coating, people while antibiont dirt material is studied also are increasingly turned to pay attention to problem of environmental pollution.
In order to reduce environmental pollution, on the one hand, be attempted to using hypotoxicity coating or non-toxic coating come instead
Front coating product, but due to being restricted by high cost and low anti-fouling performance, be not yet widely applied.On the other hand,
Some researchs show that the geometrical pattern of coating surface can effectively improve the anti-fouling performance of coating.This patent is based on this point, using light
The method that polymerization is combined with mask, is prepared for one layer of pattern type anti-tartar coating with one fixed width striped in material surface,
Effectively improve the anti-fouling performance of coating.This patent devises three kinds of polymer coatings with different anti-tartar functional groups, respectively
Referred to as sulfobetaines coating, polyethylene glycol coating and fluorine-containing coat.Wherein, sulfobetaines type coating is had good based on which
Good anti-protein adsorption ability, while and there is temperature, salinity doubling sensitivity, therefore, the research in recent years is relatively enlivened；
The anti-fouling performance of polyethylene glycol coating is known already, and it can prevent the absorption of nonspecific proteins and cell, early
Just there are many basic research in the nineties in last century, there is good application prospect in biomedical sector；And contain
Fluorine coating also becomes the anti-incrustation material that people widely pay close attention to due to its hydrophobic performance, automatical cleaning ability and antifouling capability.
The content of the invention：
It is an object of the invention to introduce a kind of method for improving coating anti-fouling performance.Same polymer is contrasted without striped
Coating, according to the stripe coating anti-tartar effect promoting prepared by the present invention.
The present invention realizes that the technical scheme of purpose is as follows：
A kind of preparation method of stripe anti-tartar coating, it is characterised in that：The antibiont dirt coating surface structure is polymerization
Thing and the alternate stripe structure of base material, pattern replaces for convex-concave, width is consistent, and range of coat thicknesses is between 100-300nm；
Preparation method is comprised the following steps：(1) monomer with antibiont dirt function is made into into monomer solution, is filled a prescription as follows:With anti-
The mass fraction of the monomer of biofouling function is 30～40, the mixed solvent 50～90, initiator of ethanol or second alcohol and water composition
0.3～0.4, crosslinking agent 1～2；Monomer with antibiont dirt function is (methyl) acrylic acid with zwitterion functional group
Ester or (methyl) acrylamide monomers, or polyethylene glycol (methyl) acrylate, or fluorine replacement (methyl) acrylic acid
The monomer of ester structure；(2) be sequentially stacked and compress according to the order of mask, PET film, base material, above-mentioned monomer solution is drawn to PET
In the gap of film and base material；Exposure 5-10 minutes, wherein light intensity are 20-40mw/cm2。
Further, the monomer with antibiont dirt function for being used is methacryloylethyl sulfobetaines or first
Epoxide polyethylene glycol methacrylate-styrene polymer or perluorooctyl acrylate.
Further, the initiator is 2- hydroxy-2-methyl -1- phenyl -1- acetone, and the crosslinking agent is trihydroxy methyl third
Alkane triacrylate.
Further, drawn in gap of the above-mentioned monomer solution to PET film with base material by capillary.
Further, the Stripe Size scope of the mask for being used is 1-20 microns.
Further, the Stripe Size of anti-L929 cell adherences is 6 microns.
Further, the PET film used in which is the transparent membrane that thickness is 80-160 μm.
Especially, it should be noted that, the striped of different in width need to be used for various sizes of biofouling, coating is lifted
The anti-fouling performance of itself.The Main Ingredients and Appearance of coating is respectively the polymethyl acyl ethyl sulfobetaines of photocuring, poly- methoxy
Base polyethylene glycol methacrylate-styrene polymer, ten trifluoro monooctyl ester of polyacrylic acid.
More specifically：Comprise the following steps：(1) by the monomer wiring solution-forming with antibiont dirt functional group, fill a prescription as follows
(2) precuring sample, exposure are prepared by the processing method of PET film protection, mask striped and capillary diffusion
5-10 minutes, wherein light intensity are 20-40mw/cm2。
Wherein, the feature of the monomer with antibiont dirt function for being used is (methyl) with zwitterion functional group
Acrylate or (methyl) acrylamide monomers, or polyethylene glycol (methyl) acrylate, or fluorine replacement (methyl)
The monomer of acrylate structural.
The wherein processing method used by precuring sample is specially and is sequentially stacked according to the order of mask, PET film, base material
And compress, monomer is diffused in gap of the PET film with base material by capillarity.
PET film used in which is the transparent membrane that thickness is 80-160 μm.
The Stripe Size of the mask used in which is 1-20 microns, and the Stripe Size of optimal anti-L929 cell adherences is 6
Microns.General width of fringe suggestion is less than cell size.
The method combined with photopolymerization using mask by the present invention, by three kinds of polymer coatings (polymethyl acyl ethyl sulphur
Ten trifluoro monooctyl ester of base glycine betaine or polymethoxy polyethylene glycol methacrylate-styrene polymer or polyacrylic acid) it is solidificated in surface substrate
Striped is gone up and formed, strengthens its anti-fouling performance by the surface characteristic of striped.In the present invention, initiator, content of crosslinking agent are determined
Coating layer thickness and anti-fouling performance, when initiator content is extremely low, polymer reaction is incomplete, it is impossible to form effective coating, draw
Send out agent content it is too high when, in coating, the molecular weight of polymer is reduced, and coating layer thickness is thinning, and anti-fouling performance declines.Content of crosslinking agent
When too low, coating adhesion is poor, thickness of thin, it is impossible to form effective coating.When crosslinking agent is too high, reduces anti-tartar polymer and exist
Content in figure layer, anti-fouling performance decline.Range of coat thicknesses advises that anti-fouling performance is preferable between 100-300nm.The present invention
Used in PET film play a part of protection, this is that PET film can protect due to coating viscosity increase in the curing process
Mask is not directly contacted with the big coating of viscosity, while the striped of coating can also be made more complete during preparation.
Description of the drawings
In Fig. 1 a embodiments 1, L929 cells are adsorbed in the optical microscope photograph of base material.
In Fig. 1 b embodiments 1, L929 cells are adsorbed in the optical microscope photograph of estriate coating.
In Fig. 1 c embodiments 1, L929 cells are adsorbed in the optical microscope photograph of the coating of 6 microns of stripeds.
Fig. 1 d base materials, without striped polymethyl acyl ethyl sulfobetaines coating, 6 microns of polymethyl acyl ethyl sulphurs
The L929 cell adsorbance statistical charts of base glycine betaine coating.
In Fig. 2 a embodiments 2, L929 cells are adsorbed in the optical microscope photograph of base material.
In Fig. 2 b embodiments 2, L929 cells are adsorbed in the optical microscope photograph of estriate coating.
In Fig. 2 c embodiments 2, L929 cells are adsorbed in the optical microscope photograph of the coating of 6 microns of stripeds.
Fig. 2 d base materials, without striped polymethoxy polyethylene glycol methacrylate-styrene polymer coating, 6 microns of polymethoxy polyethylene glycol
The L929 cell adsorbance statistical charts of methacrylate coating.
In Fig. 3 a embodiments 3, L929 cells are adsorbed in the optical microscope photograph of base material.
In Fig. 3 b embodiments 3, L929 cells are adsorbed in the optical microscope photograph of estriate coating.
In Fig. 3 c embodiments 3, L929 cells are adsorbed in the optical microscope photograph of the coating of 6 microns of stripeds.
Fig. 3 d base materials, without ten trifluoro monooctyl ester coating of striped polyacrylic acid, 6 micron polypropylenes, ten trifluoro monooctyl ester coatings of acid
L929 cell adsorbance statistical charts.
Specific embodiment
Below by embodiment is embodied as, the invention will be further described, following examples be it is descriptive, no
It is determinate, it is impossible to which protection scope of the present invention is limited with this.
Embodiment 1：
Monomer solution configuration step：3g methacryloylethyl sulfobetaine monomers are dissolved in into 5mL ethanol/2mL water
In mixed solvent, seal in darkroom ultrasound 10 minutes so as to it is dispersed in a solvent, after dispersed, in darkroom
Under environment, add the trimethylolpropane trimethacrylate of 1173 type initiators and 0.2g of 0.03g as crosslinking agent, mixing is equal
It is even that monomer solution is obtained.
Stripe coat curing steps：Order according to mask, PET film, base material is sequentially stacked and compresses, by capillary
Capillarity draw above-mentioned monomer solution and be expelled to mask and PET film gap, be positioned over after monomer diffusion completely solid
Change in case, mask plane rushes at ultraviolet source, the width of fringe of the mask for being used is 6 μm, is exposed 5 minutes under ultraviolet light,
Light intensity is 20mw/cm2.After the completion of solidification, PET film is taken off and with alcohol flushing 3 times, nitrogen is dried up and can obtain anti-with stripe
Dirty coating.The coating for obtaining is carried out into cell adherence test, control comparisons is done commonly not deal with base material.
Cell adherence testing procedure：By antibiont dirt coating and base material ultraviolet disinfection 30 minutes, sample is immersed into phosphorus
Balance 2 hours in acid buffering solution PBS, then take out and put in the nutrient solution equipped with L929 l cells, made
Culture medium is DMEM, and cell concentration is 3000cell/mL.Carry out in the CO2 incubators that 37 DEG C of volume fractions are 5%
Culture, incubation time are 1 day, by sample taking-up phosphate buffer solution drip washing three times, are 5% glutaraldehyde solution with mass fraction
Fixed cell 10h, takes out afterwards and is placed on slide, carry out observation by light microscope and take pictures.Multiplication factor is 200 times,
Randomly select 5 points to be taken pictures.The quantity of adherent cell under 1000 μ m, 1000 μm of areas is counted, what is used is soft
Part is imageJ, and the cell adsorbance for obtaining is made block diagram, and experimental result is as shown in Figure 1.
Embodiment 2：The monomer that 3g contains methoxy polyethylene glycol methacrylate-styrene polymer is dissolved in the alcohol solvent of 7mL,
Sealing in darkroom ultrasound 10 minutes so as to it is dispersed in a solvent, after dispersed, in the environment of darkroom, add
The trimethylolpropane trimethacrylate of the 1173 type initiators and 0.15g of 0.04g is well mixed and list is obtained as crosslinking agent
Liquid solution.
Stripe coat curing steps：Order according to mask, PET film, base material is sequentially stacked and compresses, by capillary
Capillarity draw above-mentioned monomer solution and be expelled to mask and PET film gap, be positioned over after monomer diffusion completely solid
Change in case, mask plane rushes at ultraviolet source, the width of fringe of the mask for being used is 6 μm, is exposed 8 minutes under ultraviolet light,
Light intensity is 30mw/cm2.After the completion of solidification, PET film alcohol flushing 3 times is taken off, nitrogen is dried up and can be obtained with stripe anti-tartar
Coating.The coating for obtaining is carried out into cell adherence test, control comparisons is done commonly not deal with base material.
Cell adherence testing procedure：, with embodiment 1, experimental result is as shown in Figure 2 for step.
Embodiment 3：The monomer that 4g contains perluorooctyl acrylate is dissolved in the alcohol solvent of 6mL, is sealed in darkroom
Middle ultrasonic 10 minutes so as to it is dispersed in a solvent, after dispersed, in the environment of darkroom, add 0.35g 1173
The trimethylolpropane trimethacrylate of type initiator and 0.1g is well mixed and monomer solution is obtained as crosslinking agent.
Stripe coat curing steps：Order according to mask, PET film, base material is sequentially stacked and compresses, by capillary
Capillarity draw above-mentioned monomer solution and be expelled to mask and PET film gap, be positioned over after monomer diffusion completely solid
Change in case, mask plane rushes at ultraviolet source, the width of fringe of the mask for being used is 6 μm, is exposed 10 minutes under ultraviolet light,
Light intensity is 40mw/cm2.After the completion of solidification, PET film alcohol flushing 3 times is taken off, nitrogen is dried up and can be obtained with stripe anti-tartar
Coating.The coating for obtaining is carried out into cell adherence test, control comparisons is done commonly not deal with base material.
Cell adherence testing procedure：, with embodiment 1, experimental result is as shown in Figure 3 for step.
Claims (7)
1. the preparation method of a kind of stripe antibiont dirt coating, it is characterised in that：The antibiont dirt coating surface structure is poly-
Compound and the alternate stripe structure of base material, pattern be convex-concave replace, width it is consistent, range of coat thicknesses 100-300nm it
Between；Preparation method is comprised the following steps：(1) monomer with antibiont dirt function is made into into monomer solution, is filled a prescription as follows:Have
The mass fraction of the monomer of antibiont dirt function is 30～40, the mixed solvent 50～90 of ethanol or second alcohol and water composition, initiation
Agent 0.3～0.4, crosslinking agent 1～2；Monomer with antibiont dirt function is (methyl) propylene with zwitterion functional group
Acid esters or (methyl) acrylamide monomers, or polyethylene glycol (methyl) acrylate, or fluorine replacement (methyl) propylene
The monomer of acrylate structure；(2) it is sequentially stacked and compresses according to the order of mask, PET film, base material, draws above-mentioned monomer solution and arrive
In the gap of PET film and base material；Exposure 5-10 minutes, wherein light intensity are 20-40mw/cm2。
2. the preparation method of a kind of stripe antibiont dirt coating according to claim 1, it is characterised in that：The tool for being used
The monomer for having antibiont dirt function is methacryloylethyl sulfobetaines or perluorooctyl acrylate.
3. the preparation method of a kind of stripe antibiont dirt coating according to claim 1, it is characterised in that：The initiator
For 2- hydroxy-2-methyl -1- phenyl -1- acetone, the crosslinking agent is trimethylolpropane trimethacrylate.
4. the preparation method of a kind of stripe antibiont dirt coating according to claim 1, it is characterised in that：By capillary
Draw in gap of the above-mentioned monomer solution to PET film with base material.
5. the preparation method of a kind of stripe antibiont dirt coating according to claim 1, it is characterised in that：What is used covers
The Stripe Size scope of mould is 1-20 microns.
6. the preparation method of a kind of stripe antibiont dirt coating according to claim 5, it is characterised in that：Anti- L929 cells
The Stripe Size of adhesion is 6 microns.
7. the preparation method of a kind of stripe antibiont dirt coating according to claim 1, it is characterised in that：Used in which
PET film be that thickness is 80-160 μm of transparent membrane.
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| CN109401657A (en) * | 2018-10-11 | 2019-03-01 | 斯迪克新型材料（江苏）有限公司 | For camber display screen can heavy industry rupture pressure disc |
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| US8288472B2 (en) * | 2009-12-29 | 2012-10-16 | Chung-Yuan Christian University | Antibiofouling nonionic-zwitterionic copolymer |
| US9403300B2 (en) * | 2010-04-14 | 2016-08-02 | 3M Innovative Properties Company | Patterned gradient polymer film and method |
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| CN107617126A (en) * | 2017-08-11 | 2018-01-23 | 天津大学 | A kind of surface modification method of porous material and application |
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