CN104212320A - Bionically textured material capable of preventing algae attachment and preparation method thereof - Google Patents
Bionically textured material capable of preventing algae attachment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a bionically textured material capable of preventing the algae attachment and a preparation method thereof. The bionically textured organic silicon modified acrylic polyurethane antifouling material is prepared by taking natural substances namely biological cuticle or leaves such as crab shell, lotus leaf, and the like as the template, and an organic silicon elastomer as the transition template. The obtained textured antifouling layer has a micrometer level protrusions or pits, wherein the protrusions or pits all have a nano structure, thus the water drop is not easy to wet the surface of the material, and fouling organisms cannot easily attach themselves to the surface of the material; at the same time, the contact surface between the fouling organisms and the bionically textured material is greatly reduced, the attachment sites are reduced, and thus attachment on the surface becomes more difficult for the fouling organisms. The natural antifouling characteristics of biological cuticle or leaves in nature are fully utilized, the characteristics of the microstructure on the surface is utilized to prevent fouling, pollution to the natural environment is not generated, and thus the material is a novel high efficient environment-friendly antifouling material.
Description
Technical field
The present invention relates to marine anti-pollution technical field, particularly relate to a kind of bionical textured material with algae-resistant adhesion property and preparation method thereof.
Background technology
There are a large amount of marine organisms in ocean environment, these marine organisms can form biodeterioration being in for a long time the facility in ocean environment with equipment surface attachment.As barnacle, algae, oyster, mussel, lime worm, Enteromorpha, Ascidian, sea anemone etc., in the adhesion of non-selectivity ground big area and the deposition on the surface such as ship housing, marine structure, aquaculture net cage, result in serious financial loss and potential safety hazard.Increasing as caused ship resistance, increasing fuel oil consumption; Cause line clogging, destroy the corrosion protection coating of building surface, cause corrosion failure.The stained controlling way of current biotinylated biomolecule mainly reaches antifouling effect by adding the material such as organotin, Red copper oxide, this kind of material has strong toxic action to attachment sea organisms, but also can cause murder by poisoning to fish, shellfish simultaneously, and can accumulate in vivo, very large impact is caused on marine biological environment, organotin is disabled in 2008, and Red copper oxide is also progressively prohibited from using.Therefore the anti-soil technology of development of new non-toxic efficient becomes most important.
The scientist of the U.S., Germany and Britain has observed the epidermal structure of the large ocean such as shark, dolphin animal, there is micron order groove in the surface of these epidermises, mucus can be secreted simultaneously, such special construction can stop the attachment of marine life, scientists is finding the method that suitable chemical means simulates these biological surface structures always, and also makes some progress.As Washington, DC university chemistry professor Karen L.Wooley has by preparing profile and the tissue that the hydrophobic of microphase-separated and oleophobic amphiphilic polymers imitate dolphin skin, seek the method regulating biology system and synthetic material interphase interaction, design can hinder the chemical functionalities group of biological attachment to simulate the skin of dolphin.The Antonia Kesel of Germany and Ralph professor Liedert study and have synthesized a kind of " shark skin ", and low-surface-energy material is selected in certification, surface has protruding span material and can reduce the attachment of most barnacle, if make this kind of material epidermis with the speed of 5-6 mile per hour at water exercise, almost the attachment of removable any biology.
Hydrolyzable silicone oil acrylic resin, the modified silicone resin containing antifouling activity functional group, methyl silicon resin, triethylene tetramine are obtained anti-fouling material by patent 200810093373.2, are formed and have regular concave-convex micro-structure surface; Patent 200910018937.0 first utilizes containing hydrogen silicone oil and (methyl) allyl acrylate Si―H addition reaction, synthesis is containing the organosilicon component of polymerizable double bond, carry out free-radical polymerized with vinyl cyanide, acrylic ester monomer again, formed hinge have the acrylate resin mixed solution of silicon gel particulate again with mixed with resin after film form spherical protuberances micro-structure surface anti-fouling material; Devise a kind of dimension-adjustable porous micro-structured surface antifouling material in patent 201110256062.5, under room temperature condition, form the micro-knot of yardstick adjustable multi-hole by acid-organosilicon crylic acid copolymer resins and amine nucleation accelerating agent and solidifying agent.Patent 201110376218.3 etches the microstructure with cruciform pattern on photomask, and elementary cell is cross column, and end is tapered, staggered, forms array; Then at the dark silicon etching process of silicon chip surface using plasma, form the microstructure of prescribed depth, method that mould copies is prepared into microstructure anti-fouling material to adopt polydimethylsiloxane to turn over.
Therefore, by bionic method, find suitable anti-fouling material, utilize the epidermal structure of chemical means to some marine animals to imitate, give coating with special surface property, as surface energy, surface modulus and surface topography etc., effectively can prevent and kill off the attachment of fouling organism.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of bionical textured material of algae-resistant adhesion property, this bionical textured material can suppress the algae marine lifes such as boat-shaped algae and Closterium to form biodeterioration being in the facility surface attachment in ocean environment for a long time preferably.
For achieving the above object, the present invention for template with crude substance such as biological epidermis or blade such as crab shell, lotus leaves, selects silicone elastomer as transition template, obtains bionical texturing organosilicon-modified acrylic urethane anti-fouling material.
A preparation method for the bionical textured material of algae-resistant adhesion property, comprises the following steps:
(1) biological template pre-treatment: cleaning biological template, and dry up;
(2) there is the silicone elastomer Template preparation of anti-pattern: by the mixture at room temperature Procuring 1 ~ 5h of polydimethylsiloxane prepolymer body and linking agent, and remove the bubble in mixed solution; Then this mixture is cast in biological template surface, at 50 ~ 150 DEG C, solidifies 8 ~ 15h; The silicone elastomer template formed after solidification is peeled off from biological template, obtains the silicone elastomer template with anti-pattern;
(3) there is the silicone elastomer Template preparation of positive pattern: the biological template had in the silicone elastomer template replacement step (2) of anti-pattern obtained with step (2), adopt the method identical with step (2) to prepare the silicone elastomer template with positive pattern;
(4) there is the bionical texturing coating preparation of positive pattern: organosilicon modified crylic acid resin, polyisocyanates and organic solvent are fully mixed, leave standstill the bubble removed in mixed solution, what then mixed solution is cast in that step (2) obtains has in the silicone elastomer template of anti-pattern, 8-18h is solidified at 50 ~ 150 DEG C, the coating formed after solidification is peeled off from silicone elastomer template, obtains the bionical texturing coating with positive pattern;
(5) there is the bionical texturing coating preparation of anti-pattern: in the silicone elastomer template with positive pattern that step (3) obtains, adopt the method identical with step (4) to prepare the bionical texturing coating with anti-pattern.
Biological template described in the present invention is animal cuticle or the plant leaf that surface has the micro-nano diadactic structure of projection and depression.Research finds: in ocean the animal such as shark, dolphin why its epidermis there is very excellent fouling resistance performance, except the chemical mucus of Surface Microtexture, secretion, also with it in ocean environment faster the speed of parading be undivided.And maritime facilities and building are static, speed of not parading, so the plant selecting that creep speed is slower or static.Therefore, further preferably, described biological template is crab shell or lotus leaf.
In step (2), the mass ratio of polydimethylsiloxane prepolymer body and linking agent is 10:1, and mixed solution has the transparent elastomer of toughness by being solidified into, namely described silicone elastomer template.
The invention is intended to be reacted by isocyanate functional group-N=C=O and hydroxyl-OH by organosilicon modified crylic acid resin and polyisocyanates generate polyurethane structural, in the generative process of urethane, the properity impact of NCO/OH comparison synthetic product is fairly obvious.The viscosity of emulsion reduces along with the increase of NCO/OH ratio.This is because NCO/OH is than larger, in urethane, hard section (being made up of polyisocyanates or small molecule chain extender) content raises, and soft section of (being usually made up of polyethers or polyester) content is relatively low.The elasticity of such urethane just reduces, and tensile strength raises.After considering, in organosilicon modified crylic acid resin and polyisocyanates, the mol ratio of NCO/OH is 0.8 ~ 1.2:1 in preferred steps (4).Wherein, polyisocyanates can select hexamethylene diisocyanate (HDI) tripolymer, toluene diisocyanate trimer etc.
Organic solvent described in step (4) is aromatic solvent, and its usage quantity is 20% ~ 60% of organic-silicon-modified Hydroxylated acrylic resin and polyisocyanates total mass.Resin can fully be dissolved in organic solvent.
Present invention also offers the bionical textured material with algae-resistant adhesion property that above-mentioned preparation method obtains.
The present invention with crude substance such as biological epidermis or blade such as crab shell, lotus leaves for template, using silicone elastomer as transition template, prepare the organosilicon-modified acrylic urethane texturing antifouling coating that surface has micro-nano diadactic structure, this coating has micron-sized projection or pit, projection or pit have nanostructure, enhance the nonwetting character of water droplet at material surface, thus make fouling organism also be not easy attachment; Greatly reduce the contact area between fouling organism and antifouling coating simultaneously, the attachment site of fouling organism is reduced, thus be not easy attachment, even if attachment also easy desorption.
The present invention utilizes nature biotechnology blade or epidermis to have natural antifouling properties, adopts the microstructure characteristic on surface to carry out antifouling, and not producing physical environment and pollute, is a kind of high-efficiency environment friendly anti-fouling material based on new approaches, new ideas.
Accompanying drawing explanation
Fig. 1 is the preparation process schematic diagram of the bionical texturing coating of the present invention;
Fig. 2 is the SEM figure of imitative crab shell positive pattern texturing coating morphology;
Fig. 3 is the SEM figure that imitative crab shell bears pattern texturing coating morphology;
Fig. 4 a is the three-dimensional appearance figure of imitative crab shell positive epidermis morphology texturing coating;
Fig. 4 b is the three-dimensional appearance figure that imitative crab shell bears epidermis morphology texturing coating;
Fig. 5 is the SEM observation figure of imitative lotus leaf positive pattern texturing coating morphology;
Fig. 6 is the SEM observation figure that imitative lotus leaf bears pattern texturing coating morphology;
Fig. 7 a is the three-dimensional appearance figure of imitative lotus leaf positive pattern texturing coating;
Fig. 7 b is the three-dimensional appearance figure that imitative lotus leaf bears pattern texturing coating;
Fig. 8 is the laser confocal microscope figure of the imitative crab shell coating before and after the attachment of boat-shaped algae;
Fig. 9 is the laser confocal microscope figure of the imitative crab shell coating before and after Closterium attachment;
Figure 10 is the laser confocal microscope figure of the imitative lotus leaf coating before and after the attachment of boat-shaped algae;
Figure 11 is the laser confocal microscope figure of the imitative lotus leaf coating before and after Closterium attachment.
Embodiment
Embodiment 1: the preparation of imitative crab shell positive pattern microstructure organic silicon acrylic ester antifouling coating
There is according to the preparation of flow process shown in Fig. 1 the texturing coating of the positive pattern of crab shell: deionized water ripples and washes crab shell surface, and dries up by faint nitrogen gas stream.Then prepare silicone elastomer template; Preparation process is as follows: the ratio of DOW CORNING SYLGARD184 polydimethylsiloxane (PDMS) and its supporting linking agent 10:1 in mass ratio fully mixed, first solidify 2h at ambient temperature, and remove the bubble in mixed solution; Then mixed solution is poured on crab shell surface, then solidifies 12h at 70 DEG C; Finally the PDMS after solidification is peeled off from crab shell, namely obtain the silicone elastomer template with the negative pattern in crab shell surface.
Prepare organosilicon-modified acrylic polyurethane coating process as follows: by organosilicon modified crylic acid resin (SKD002, hydroxy radical content 1.9%) with hexamethylene diisocyanate trimer (NCO content 18%) and dimethylbenzene in mass ratio 3:1:1.5 fully mix (NCO/OH mol ratio 1.2:1), leave standstill 20min, and remove the bubble in mixed solution; Then mixed solution is poured on and there is crab shell bears in the silicone elastomer template of pattern, 12h is solidified again at 70 DEG C, finally the coating formed after solidification is peeled off from silicone elastomer template, obtain the bionical texturing coating of organosilicon-modified acrylate with the positive pattern of crab shell.
As shown in Figure 2, from a to d, enlargement ratio increases successively.It is protruding to there is regularly arranged hangnail in imitative positive crab shell texturing coatingsurface, finds that hangnail size is basically identical by measuring, and the diameter of hangnail bottom is 1.5 μm (as shown in d in Fig. 2) left and right.And these hangnails arrangement very regular (as shown in b in Fig. 2), be roughly close-packed hexagonal structure.Distance between hangnail is all at about 6.5 μm, and variation range is little, substantially between 5.5 μm to 7.5 μm.The height being imitated hangnail projection in crab shell positive pattern texturing coating texturing coating by Fig. 4 a is as seen about 4 μm, and by AFM software analysis, the surfaceness of imitative crab shell positive pattern texturing coating is 0.62 μm.
Embodiment 2: imitative crab shell bears the preparation of pattern microstructure organic silicon acrylic ester antifouling coating material
Have according to the preparation of flow process shown in Fig. 1 the texturing coating that crab shell bears pattern, the temperature and time wherein solidified can suitably regulate: ripple with deionized water and wash crab shell surface, and dry up by faint nitrogen gas stream.Then prepare silicone elastomer template; Preparation process is as follows: the ratio of DOW CORNING SYLGARD184 polydimethylsiloxane (PDMS) and its supporting linking agent 10:1 in mass ratio fully mixed, first solidify 2h at ambient temperature, and remove the bubble in mixed solution; Then mixed solution is poured on crab shell surface, then solidifies 15h at 50 DEG C; Finally the PDMS after solidification is peeled off from crab shell, namely obtain the silicone elastomer template with the negative pattern in crab shell surface.PDMS mixed solution after process is poured into the template silicone elastomer template with the negative surface topography in crab shell surface obtaining having the positive pattern in crab shell surface.
Prepare organosilicon-modified acrylic polyurethane coating process as follows: by organosilicon modified crylic acid resin (SKD002, hydroxy radical content 1.9%) with hexamethylene diisocyanate trimer (NCO content 18%) and dimethylbenzene in mass ratio 3.5:1:1.5 fully mix (NCO/OH mol ratio 1:1), leave standstill 20min, and remove the bubble in mixed solution; Then mixed solution is poured on there is the positive pattern in crab shell surface PDMS template on, 16h is solidified again at 50 DEG C, finally the coating formed after solidification is peeled off from silicone elastomer template, obtain that there is the bionical texturing coating of organosilicon-modified acrylate that crab shell bears pattern.
Prepared copies the SEM observation figure of the bionical texturing organosilicon acroleic acid polyurethane coating of the negative pattern in Blue Swimming Crab shell surface as indicated at 3.From a to d, enlargement ratio increases successively.Corresponding imitative crab shell is born pattern texturing coatingsurface and be there is regularly arranged pit, is about 1.5 μm by measuring the diameter finding pit top, same, and the arrangement of these pits is in close-packed hexagonal structure.Distance between pit is about 6.5 μm.Be about 1 μm by Fig. 4 b degree of depth that imitative crab shell bears pit in pattern texturing coating as seen, by AFM software analysis, the surfaceness of imitative negative crab shell texturing coating is 0.08 μm.
Embodiment 3: the preparation of imitative lotus leaf positive pattern microstructure organic silicon acrylic ester antifouling coating material
Have the texturing coating of the positive pattern of lotus leaf according to the preparation of flow process shown in Fig. 1, the temperature and time wherein solidified can suitably regulate: ripple with deionized water and wash lotus leaf surface, and dries up by faint nitrogen gas stream.Then prepare PDMS template; Preparation process is as follows: the ratio of DOW CORNING SYLGARD184 polydimethylsiloxane (PDMS) and its supporting linking agent 10:1 in mass ratio fully mixed, first solidify 2h at ambient temperature, and remove the bubble in mixed solution; Then mixed solution is poured on lotus leaf surface, then solidifies 8h at 150 DEG C; Finally the silicone elastomer after solidification is peeled off from lotus leaf, namely obtain that there is the silicone elastomer template that lotus leaf surface bears pattern.
Prepare organosilicon-modified acrylic polyurethane coating process as follows: by organosilicon modified crylic acid resin (SKD002, hydroxy radical content 1.9%) with toluene diisocyanate trimer (NCO content 8%) and toluene in mass ratio 2.1:1:1.5 fully mix (NCO/OH mol ratio 0.8:1), leave standstill 20min, and remove the bubble in mixed solution; Then mixed solution is poured on and there is lotus leaf bears in the silicone elastomer template of pattern, 6h is solidified again at 150 DEG C, finally the coating formed after solidification is peeled off from silicone elastomer template, obtain the bionical texturing coating of organosilicon-modified acrylic urethane with the positive pattern of lotus leaf.
As shown in Figure 5, from a to c, enlargement ratio increases the SEM figure of the bionical texturing organosilicon acroleic acid polyurethane coating of imitative lotus leaf front surface pattern successively.Scheming us according to SEM and find that imitative lotus leaf positive pattern texturing coatingsurface exists the mastoid process of irregular alignment, be about 7.5 μm, but mastoid process size is not quite identical by measuring the diameter finding mastoid process bottom.And the intermastoid distance of these irregular alignments is substantially all between 9-11 μm, but a small amount of intermastoid distance is also had to be less than 3 μm or be greater than 15 μm.The height being imitated mastoid process in lotus leaf positive pattern texturing coating texturing coating by Fig. 7 a is as seen about 8 μm, and by AFM software analysis, the surfaceness that we can imitate lotus leaf positive pattern texturing coating is 2.47 μm.
Embodiment 4: imitative lotus leaf bears the preparation of pattern microstructure organic silicon acrylic ester antifouling coating material
Have according to the preparation of flow process shown in Fig. 1 the texturing coating that lotus leaf bears pattern, the temperature and time wherein solidified can suitably regulate: ripple with deionized water and wash lotus leaf surface, and dries up by faint nitrogen gas stream.Then prepare PDMS template; Preparation process is as follows: the ratio of DOW CORNING SYLGARD184 polydimethylsiloxane (PDMS) and its supporting linking agent 10:1 in mass ratio fully mixed, first solidify 2h at ambient temperature, and remove the bubble in mixed solution; Then mixed solution is poured on lotus leaf surface, then solidifies 10h at 100 DEG C; Finally the PDMS after solidification is peeled off from lotus leaf, namely obtain that there is the silicone elastomer template that lotus leaf surface bears pattern.PDMS mixed solution after process is poured into the template having and PDMS template that lotus leaf surface bears surface topography obtains having the positive pattern of lotus leaf surface.
Prepare organosilicon-modified acrylate coating procedure as follows: by organosilicon modified crylic acid resin (SKD002, hydroxy radical content 1.9%) with toluene diisocyanate trimer (NCO content 8%) and toluene in mass ratio 1.7:1:1.5 fully mix (NCO/OH mol ratio 1:1) and leave standstill 20min, and remove the bubble in mixed solution; Then mixed solution is poured in the silicone elastomer template with the positive pattern of lotus leaf surface, 10h is solidified again at 100 DEG C, finally the coating formed after solidification is peeled off from silicone elastomer template, obtain that there is the bionical texturing coating of organosilicon-modified acrylic urethane that lotus leaf bears pattern.
Prepared lotus leaf surface of copying bears the SEM of the bionical texturing organosilicon acroleic acid polyurethane (hereinafter referred to as imitative load leaf texturing coating) of pattern as shown in Figure 6.From a to c, enlargement ratio increases successively.There is the pit of irregular alignment in corresponding imitative load leaf texturing coatingsurface, is about 7.5 μm by measuring the diameter finding pit top.Same, pit size is not quite identical, and the distance great majority between the pit of these irregular alignments are all between 9-11 μm.Be about 8 μm by Fig. 7 b degree of depth that imitative lotus leaf bears pit in pattern texturing coating as seen, by AFM software analysis, the surfaceness that imitative lotus leaf bears pattern texturing coating is 1.81 μm.
Performance test:
(1), the anti-algae adhesion detection of antifouling coating in embodiment 1,2
Relative to without textured coating (a and a '), the imitative positive crab shell texturing coating of embodiment 1 and 2 (b and b ') and the imitative negative textured coating of crab shell (c and c ') all there is good anti-fouling effect to boat-shaped algae, the preventive effect of boat-shaped algae is more or less the same, as shown in Figure 8, the reduced rate of adhesion amount is respectively 69% and 70% to the laser co-focusing photo of boat-shaped algae adhesion amount.The laser co-focusing photo of Closterium adhesion amount as shown in Figure 9, relative to without textured coating (a and a '), imitative positive crab shell texturing coating (b and b ') and the imitative negative textured coating of crab shell (c and c ') also all there is good anti-fouling effect to Closterium, adhesion amount reduced rate is respectively 68% and 65%.
(2), the anti-algae adhesion detection of embodiment 3,4 antifouling coating
Imitative lotus leaf positive and negative pattern microstructure organic silicon acrylic ester antifouling coating in embodiment 3 and 4 to the confocal laser scanning microscope figure after the attachment of boat-shaped algae as shown in Figure 10, imitative lotus leaf positive/negative pattern texturing coating has good anti-fouling effect to boat-shaped algae, and, imitative load leaf texturing coating (c and c ') adhesion amount reduced rate is 74%, be better than imitative positive lotus leaf texturing coating (b and b ', adhesion amount reduced rate 54%).The contact angle of imitative lotus leaf positive/negative pattern texturing coatingsurface water all can reach 113 °.The laser confocal microscope figure of the imitative lotus leaf coating after Closterium attachment as shown in figure 11, the texturing coating (being respectively b and b ', c and c ') of the imitative positive/negative pattern of lotus leaf also has good anti-fouling effect to Closterium, and adhesion amount reduced rate can reach 74% and 73% respectively.
Claims (7)
1. there is a preparation method for the bionical textured material of algae-resistant adhesion property, it is characterized in that, comprise the following steps:
(1) biological template pre-treatment: cleaning biological template, and dry up;
(2) there is the silicone elastomer Template preparation of anti-pattern: by the mixture at room temperature Procuring 1 ~ 5h of polydimethylsiloxane prepolymer body and linking agent, and remove the bubble in mixed solution; Then this mixture is cast in biological template surface, at 50 ~ 150 DEG C, solidifies 8 ~ 15h; The silicone elastomer template formed after solidification is peeled off from biological template, obtains the silicone elastomer template with anti-pattern;
(3) there is the silicone elastomer Template preparation of positive pattern: the biological template had in the silicone elastomer template replacement step (2) of anti-pattern obtained with step (2), adopt the method identical with step (2) to prepare the silicone elastomer template with positive pattern;
(4) there is the bionical texturing coating preparation of positive pattern: organosilicon modified crylic acid resin, polyisocyanates and organic solvent are fully mixed, leave standstill the bubble removed in mixed solution, what then mixed solution is cast in that step (2) obtains has in the silicone elastomer template of anti-pattern, 8-18h is solidified at 50 ~ 150 DEG C, the coating formed after solidification is peeled off from silicone elastomer template, obtains the bionical texturing coating with positive pattern;
(5) there is the bionical texturing coating preparation of anti-pattern: in the silicone elastomer template with positive pattern that step (3) obtains, adopt the method identical with step (4) to prepare the bionical texturing coating with anti-pattern.
2. the preparation method with the bionical textured material of algae-resistant adhesion property according to claim 1, is characterized in that, described biological template is animal cuticle or the plant leaf that surface has the micro-nano diadactic structure of projection and depression.
3. the preparation method with the bionical textured material of algae-resistant adhesion property according to claim 2, is characterized in that, described biological template is crab shell or lotus leaf.
4. the preparation method with the bionical textured material of algae-resistant adhesion property according to claim 1, is characterized in that, in step (2), the mass ratio of polydimethylsiloxane prepolymer body and linking agent is 10:1.
5. the preparation method with the bionical textured material of algae-resistant adhesion property according to claim 1, is characterized in that, in organosilicon modified crylic acid resin and polyisocyanates, the mol ratio of NCO/OH is 0.8 ~ 1.2:1 in step (4).
6. the preparation method with the bionical textured material of algae-resistant adhesion property according to claim 1, it is characterized in that, organic solvent described in step (4) is aromatic solvent, and its usage quantity is 20% ~ 60% of organic-silicon-modified Hydroxylated acrylic resin and polyisocyanates total mass.
7. according to the bionical textured material with algae-resistant adhesion property that any one of claim 1 ~ 6 preparation method obtains.
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