CN104861755A - Novel hydrogel anti-fouling coating preparation method - Google Patents
Novel hydrogel anti-fouling coating preparation method Download PDFInfo
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- CN104861755A CN104861755A CN201510236375.2A CN201510236375A CN104861755A CN 104861755 A CN104861755 A CN 104861755A CN 201510236375 A CN201510236375 A CN 201510236375A CN 104861755 A CN104861755 A CN 104861755A
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
- C09D5/1637—Macromolecular compounds
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a novel hydrogel anti-fouling coating preparation method. PVA (polyvinyl alcohol), dimethyl sulfoxide and deionized water are mixed, stirred and completely dissolved to prepare PVA gel; 50 grams of PVA gel is placed into AAm (acrylamide) solution containing KPS and soaked to obtain hydrogel with a PVA/PAAm (polyacrylamide) dual-network structure; the hydrogel is placed into the deionized, soaked, dried, crushed, cleaned with ethanol and dried into micro-powder, epoxy resin is added into defoaming agents and rapidly stirred, the hydrogel micro-powder is blended with the epoxy resin and rapidly uniformly stirred, and then epoxy resin curing agents are added into mixture and stirred to obtain a hydrogel anti-fouling coating. The novel hydrogel anti-fouling coating preparation method has the advantage that the hydrogel anti-fouling coating is high in anti-fouling performance.
Description
Technical field
The invention belongs to compound technical, relate to a kind of novel hydrogels antifouling coating preparation method.
Background technology
Marine biofouling brings great harm to boats and ships and maritime facilities, and bionical anti-fouling method is in widespread attention because having the advantage such as safety and environmental protection and high efficiency.Utilize hydrogel material to simulate the rete malpighii of the marine organisms such as dolphin and marine fishes skin surface High water cut, low elastic modulus (softness) and low-friction coefficient to prevent marine biofouling, be considered to a kind of revolutionary novel method.But the low strength of hydrogel material and low sticking power seriously constrain its application.
Dolphin lives in the seawater all day, but its skin surface is non-cohesive any stained marine organisms, the fluff structures that research is shown to be due to its skin surface projection can continuous release hydrogel mucus, top layer can be upgraded by metabolism, remove surface adhesion thing, thus reach the effect of fouling resistance bioadhesion.
China prevents the research in biodeterioration to be in the starting stage utilizing hydrogel.Dong Jing
[23]research finds that ionic hydrogels has better anti-adhesion ability than non-ionic type hydrogel, the polychloride trimethylammonium of its cationic-3-acrylamide propyl amine (PDMAPAA-Q) hydrogel, effect is the most desirable, its Spore adhesion amount is minimum, and gametophyte number, ovulation amount and germination rate are zero, be applicable to doing anti-fouling material.Chinese Marine University and Qingdao Haiyang corrosion and protection technology national defence key lab
[24]combine the physical blending thing (COP) of polyacrylamide and silicone resin and polymkeric substance (PAS), add in silicone resin respectively and make coating, simulate shagreen rete malpighii state, there is certain anti-fouling effect.Chinese Academy of Sciences Jiang Lei
[25]seminar's research has been prepared and has been had micro-nano hierarchy, the bionic fish-skin hydrogel surface of super oleophobic property, expects the antifouling property realizing excellence.More than research does not have the antifouling mechanism of further investigated hydrogel material, does not consider the problem how solving hydrogel sticking power and intensity difference yet.Apply also far apart at this revolutionary anti-fouling material of China's hydrogel and real sea.
Summary of the invention
The object of the present invention is to provide a kind of hydrogel novel antifouling coating production, solve existing hydrogel decontamination coated material intensity and sticking power low, the problem that antifouling property is low.
The technical solution adopted in the present invention is carried out according to following steps:
Step 1, mix according to PVA, dimethyl sulfoxide (DMSO) and the deionized water quality ratio than 7:2:1, under agitation, the constant-temperature heating sleeve being placed in 100-110 DEG C dissolves completely, put in the refrigerator of-18 DEG C, freezing 20h, at room temperature thaw 4h, makes PVA gel;
Step 2,50 grams of PVA gels are put into containing KPS (the AAm solution 500mL of n (KPS)/n (AMPS)=1% soaks, AAm is made to enter in the first layer network, 24h is soaked to balance at envrionment temperature is 4 DEG C, take out subsequently and put into the container be made up of sheet glass and silica-gel plate, after reacting 15h under putting into constant temperature 50 DEG C of oxygen free conditions, obtain the hydrogel of PVA/PAAm dual network structure;
Step 3: hydrogel is put into deionized water and soak 7 days, needs timing to go to change deionized water to remove the unreacted monomer contained in gel in this process;
Step 4: after the hydrogel water suction of soaking is saturated, dry 24 hours, dried hydrogel is pulverized, with ethanol purge, put cleaning 30min in Ultrasonic Cleaners into, mainly remove the impurity such as grease on hydrogel micro mist surface, then take out dry 24 hours of constant temperature blast drying oven hydrogel micro mist being placed on 80 DEG C;
Step 5: epoxy resin 100 grams is added defoamer 0.55 gram of rapid stirring, again by blended for hydrogel micro mist 20 grams rapid stirring 20min, make mutually to mix, add epoxy curing agent 10 grams of rapid stirring 5min again, then place 5min and treat that it does not have bubble completely, obtain hydrogel antifouling coating.
The invention has the beneficial effects as follows that hydrogel decontamination coating antifouling property of the present invention is high.
Accompanying drawing explanation
Fig. 1 is absorbing water powder modified coating static immersing quality change; (a) particle diameter 0.38mm absorbing water powder; (b) particle diameter 0.25mm absorbing water powder; (c) particle diameter 0.075mm absorbing water powder;
Fig. 2 is particle diameter is 0.38mm absorbing water powder modified coating frictional coefficient comparison diagram;
Fig. 3 is particle diameter is 0.25mm absorbing water powder modified coating frictional coefficient comparison diagram;
Fig. 4 is particle diameter is 0.75mm absorbing water powder modified coating frictional coefficient comparison diagram.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
A preparation method for novel hydrogels antifouling coating, is characterized in that carrying out according to following steps:
Step 1, mix according to PVA, dimethyl sulfoxide (DMSO) and the deionized water quality ratio than 7:2:1, under agitation, the constant-temperature heating sleeve being placed in 100-110 DEG C dissolves completely, put in the refrigerator of-18 DEG C, freezing 20h, at room temperature thaw 4h, makes PVA gel;
Step 2,50 grams of PVA gels are put into containing KPS (the AAm solution 500mL of n (KPS)/n (AMPS)=1% soaks, AAm is made to enter in the first layer network, 24h is soaked to balance at envrionment temperature is 4 DEG C, take out subsequently and put into the container be made up of sheet glass and silica-gel plate, after reacting 15h under putting into constant temperature 50 DEG C of oxygen free conditions, obtain the hydrogel of PVA/PAAm dual network structure;
Step 3: hydrogel is put into deionized water soak 7d (my god), need in this process timing go change deionized water to remove the unreacted monomer contained in gel;
Step 4: after the hydrogel water suction of soaking is saturated, dry 24 hours, dried hydrogel is pulverized, with ethanol purge, put cleaning 30min in Ultrasonic Cleaners into, mainly remove the impurity such as grease on hydrogel micro mist surface, then take out dry 24 hours of constant temperature blast drying oven hydrogel micro mist being placed on 80 DEG C;
Step 5: epoxy resin 100 grams is added defoamer 0.55 gram of rapid stirring, again by blended for hydrogel micro mist 20 grams rapid stirring 20min, make mutually to mix, add epoxy curing agent 10 grams of rapid stirring 5min again, then place 5min and treat that it does not have bubble completely, obtain hydrogel antifouling coating.
The feature of subject hydrogel antifouling coating is: 1. have super hydrophilic and water absorbing properties and coating can be made to be rendered as moisture film state in the seawater, and antifouling property improves can be predicted; 2. preparation technology of coating is simple and materials safety is nontoxic, meets environmental requirement, and is applicable to the large-scale surface construction relating to extra large structure such as naval vessel and underwater facility; 3. solve the problem of hydrogel layer poor adhesive force, can in seawater scouring, the temperature difference the complicated severe ocean environment life-time service such as comparatively large and alternation of wetting and drying; 4. can be combined with the organic antifouling coating of existing high-performance, the existing anti-soil technology of high efficiency composition.
Coating performance detected result of the present invention is as shown in table 1.
Table 1
For subject hydrogel antifouling coating, prepared by compound coating, carried out screening and processing by hydrogel micro mist, carry out hydrogel micro mist and epoxy resin physical blending, encapsulated by dried sample classification, guard against damp, absorbing water powder, water-absorption fiber blending ratio are as shown in table 2.
Table 2 absorbing water powder, water-absorption fiber blending ratio
Note: P1, P2, P3, P4 are respectively hydrogel particle diameter 0.38,0.25,0.075, P0 and represent epoxy resin varnish experimental result and analysis
Absorbing water powder and epoxy resin interface bonding state are analyzed
After hydrogel micro mist buries and is overlying on epoxy resin-base, seawater slowly penetrates into coating from the Minute pores of epoxy resin surface, hydrogel water-swellable, forms low surface energy, super lubricating hydrogel sealing coat at coatingsurface.The dissolution rate of water-absorbing resin, the density forming hydrogel protective layer and peeling rate all directly affect the life-span of hydrogel anti-fouling material.The perfect condition of water-absorbing resin has solvent insensitivity, the physics-chem characteristic of itself does not affect by the cross-linking and curing reaction of epoxy resin, hydrogel can be gone out by sustained release in long period of soaking process, utilize infrared spectroscopic study coating microstrueture, the bonding state of water-absorbing resin and epoxy resin interface can be understood.
Find out from the infrared spectrogram of the micronization modified coating of different-grain diameter hydrogel, the hydrogel micro mist of the different percentage compositions of different-grain diameter does not all form new chemical bonds with epoxy resin, and is only simple physical blending.Therefore process in leaching is continued after adhering to stained thing after hydrogel micro mist water absorption and swelling not by the impact of matrix.
The dissolved corrosion research of absorbing water powder
Whether absorbing water powder water absorption and swelling affects the integrity of matrix, and form water-setting micelle compactness extent and can continue to be stored in coatingsurface, even if after surface water gel film comes off, can new hydrogel thin film continue to be formed, and this all has direct relation with the stripping of hydrogel.
The static dissolved corrosion of the micronization modified coating of hydrogel absorbing water powder modified coating static immersing quality change as Suo Shi Fig. 1 (a) to (c), Fig. 1 (a) is particle diameter 0.38mm absorbing water powder, Fig. 1 (b) is particle diameter 0.25mm absorbing water powder, and Fig. 1 (c) is particle diameter 0.075mm absorbing water powder.Upper as can be seen from figure, first different percentage composition and different-grain diameter absorbing water powder or water-absorption fiber inhaled full water at first 4 days, hydrogel quality in 4-8 days epoxy resin reduces to some extent, illustrate that some hydrogel stripping is very fast, and after 8-18 days, hydrogel quality tends to balance.Illustrate absorbing water powder and water suction fine modification coating soak in the seawater surface form hydrogel thin film can sustainable existence.From figure, can find out the difference of the component along with hydrogel micro mist, the content of the hydrogel on modified coating surface is different simultaneously.The higher absorbing water powder of content is in Blending Processes, and some is easier to the top layer remaining in matrix, and and be easy to peel off under seawater scouring after matrix combination degree poor hydrogel micro mist water absorption and swelling.But along with the passing of soak time, the hydrogel content of matrix surface just tends to balance, this is that the probability that hydrogel is combined with matrix is higher because water absorbent gel content is higher, can rely on mutually between hydrogel, to keep hydrogel long-term existence in coating.Such hydrogel thin film is just not easily peeled off by seawater.Obtain a result in particle diameter 0.38mm hydrogel micronization modified coating static immersing stripping surface from test: no matter be soak 18 days or 80 days in the seawater, along with the content of hydrogel micro mist increases, and the gel film that surface is formed is also tightr.But along with the increase of content, hydrogel micro mist easily causes coated substrate to ftracture thus destroys the integrity of matrix in water absorption and swelling process, and such matrix is easy to come off under the long souring of seawater, loses antifouling property.After having soaked 80 days in the seawater, hydrogel can also constantly stripping, coated substrate remain containing the very thin hydrogel thin film of one deck, soak after 80 days, also many all than immersion 18 days of the content of the hydrogel on matrix, this illustrate the stripping of water-absorbing resin be one uninterrupted and be continue process slowly, corresponding to its Changing Pattern and hydrogel quality change rule.
Absorbing water powder modified coating surface lubricating characteristics is studied
Hydrogel coating lubricating property (frictional coefficient) is related to the antifouling life of antifouling paint, and enough lubricating properties are the problems that must consider when designing coating.The characteristic of the hydrogel micro mist in modified coating is the basic factor determining lubricating property.Its particle diameter with hydrogel micro mist, dispersiveness and the intensity be combined with matrix have close relationship.After the hydrogel state that particularly coating water suction rear surface is formed, under the washing away of seawater, its lubricating property is directly connected to antifouling property.Therefore select suitable particle diameter and its percentage composition can be very important to the lubricating property evaluating coating.
The contrast of the micronization modified coating of particle diameter 0.38mm hydrogel frictional coefficient under load 4N as shown in Figure 2.Sample is respectively P1-3, P1-6, P1-9, P1-12.As seen from Figure 2, frictional coefficient increases along with hydrogel powder content and reduces.Wherein this group friction coefficient curve of P1-3 is larger, is because hydrogel powder content is lower, forms the surface that hydrogel thin film is difficult to cover completely whole coating after its water absorption and swelling.The smooth water absorbent gel film friction coefficient of the densification formed after this group coating water suction of P1-12 is minimum.
The contrast of the micronization modified coating of particle diameter 0.25mm hydrogel frictional coefficient under load 4N as shown in Figure 3.Sample is respectively P2-5, P2-10, P2-20, P2-30.As seen from Figure 3, frictional coefficient first reduces to increase afterwards along with content increases and decreases.Wherein the frictional coefficient of this group of P2-5 is the highest, is wherein that can not cover matrix surface completely after absorbing water powder water absorption and swelling, bistrique and matrix bad student rub, and cause frictional coefficient to increase because this group absorbing water powder comparision contents is little.Wherein the frictional coefficient of this group of P2-10 is minimum.And this group of P2-30 is why large than P2-10 frictional coefficient, is because hydrogel grain size of micropowder is comparatively large and content is higher, after such hydrogel micro mist water absorption and swelling, occurs that a part of absorbing water powder and matrix are in conjunction with untight phenomenon.Especially when too high levels can cause the cracking of matrix, namely under very little power effect, just easily there is obscission, thus cause frictional coefficient to increase.
The contrast of particle diameter 0.075mm modified coating frictional coefficient under load 4N as shown in Figure 4.Sample is respectively P3-5, P3-10, P3-15, P3-20, P3-25.Can find out, modified coating frictional coefficient first reduces rear increase along with water suction content increase.The frictional coefficient of this group of P3-25 is maximum, this is because P3-25 hydrogel powder content is maximum, after its absorbing water powder water absorption and swelling, matrix ftractures.This group frictional coefficient of P3-5 is comparatively large, is can not cover whole matrix surface completely owing to forming hydrogel after hydrogel micro mist water absorption and swelling.The frictional coefficient of this group of P3-10 is minimum.
Can draw by experiment, antifouling coating of the present invention can form the fine and close smooth hydrogel thin film of one deck.Micro-algae can be effectively suppressed to adhere to and growth such as stained thing adhesion such as real marine barnacle, Mussels etc.Water film can be formed on surface in coating immersion process, and constantly can discharge hydrogel, have and automatically upgrade cleaning capacity, can prevent marime fouling thing from adhering to, significantly improve coating antifouling property.
And experimental water gel micro mist of the present invention builds the microtexture of similar dolphin epidermis, and prepare environmental friendliness array type hydrogel antifouling coating system.Each coating is carried out to the Mechanics Performance Testings such as sound state scour resistance and surface lubricating characteristics, and the antifouling property of coating is have studied by cultivating marine microalgae and real extra large link plate under the artificial condition in laboratory, obtain conclusion as follows: the micronization modified coating of hydrogel all can form the finer and close water absorbent gel film of one deck after water absorption and swelling.But its content is higher all there is MATRIX CRACKING phenomenon.Particle diameter is less, and the certain micronization modified coating of hydrogel of content can suppress the adhesion of stained thing.Wherein hydrogel micro mist is 0.075mm content is that 15% and 20% modified coating fouling resistance physical performance is best.
The above is only to better embodiment of the present invention, not any pro forma restriction is done to the present invention, every any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (1)
1. a novel hydrogels antifouling coating preparation method, is characterized in that: carry out according to following steps:
Step 1, mix according to PVA, dimethyl sulfoxide (DMSO) and the deionized water quality ratio than 7:2:1, under agitation, the constant-temperature heating sleeve being placed in 100-110 DEG C dissolves completely, put in the refrigerator of-18 DEG C, freezing 20h, at room temperature thaw 4h, makes PVA gel;
Step 2,50 grams of PVA gels are put into containing KPS (the AAm solution 500mL of n (KPS)/n (AMPS)=1% soaks, AAm is made to enter in the first layer network, 24h is soaked to balance at envrionment temperature is 4 DEG C, take out subsequently and put into the container be made up of sheet glass and silica-gel plate, after reacting 15h under putting into constant temperature 50 DEG C of oxygen free conditions, obtain the hydrogel of PVA/PAAm dual network structure;
Step 3: hydrogel is put into deionized water and soak 7 days, needs timing to go to change deionized water to remove the unreacted monomer contained in gel in this process;
Step 4: after the hydrogel water suction of soaking is saturated, dry 24 hours, dried hydrogel is pulverized, with ethanol purge, put cleaning 30min in Ultrasonic Cleaners into, mainly remove the grease on hydrogel micro mist surface, then take out dry 24 hours of constant temperature blast drying oven hydrogel micro mist being placed on 80 DEG C;
Step 5: epoxy resin 100 grams is added defoamer 0.55 gram of rapid stirring, again by blended for hydrogel micro mist 20 grams rapid stirring 20min, make mutually to mix, add epoxy curing agent 10 grams of rapid stirring 5min again, then place 5min and treat that it does not have bubble completely, obtain hydrogel antifouling coating.
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Cited By (4)
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| CN109661442A (en) * | 2016-07-11 | 2019-04-19 | 株式会社可乐丽 | Aquatile repellent coating composition |
| CN110982226A (en) * | 2019-12-13 | 2020-04-10 | 南京信息工程大学 | Structured high-elasticity buffer composite resin material and preparation method thereof |
| CN111303716A (en) * | 2020-03-03 | 2020-06-19 | 江苏海晟涂料有限公司 | Anti-cracking and anti-fouling paint for ship bottom and preparation method thereof |
| CN115028875A (en) * | 2022-07-12 | 2022-09-09 | 哈尔滨工程大学 | Shark skin-imitated dynamic antifouling material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109661442A (en) * | 2016-07-11 | 2019-04-19 | 株式会社可乐丽 | Aquatile repellent coating composition |
| CN110982226A (en) * | 2019-12-13 | 2020-04-10 | 南京信息工程大学 | Structured high-elasticity buffer composite resin material and preparation method thereof |
| CN110982226B (en) * | 2019-12-13 | 2022-03-08 | 南京信息工程大学 | Structured high-elasticity buffer composite resin material and preparation method thereof |
| CN111303716A (en) * | 2020-03-03 | 2020-06-19 | 江苏海晟涂料有限公司 | Anti-cracking and anti-fouling paint for ship bottom and preparation method thereof |
| CN115028875A (en) * | 2022-07-12 | 2022-09-09 | 哈尔滨工程大学 | Shark skin-imitated dynamic antifouling material and preparation method thereof |
| CN115028875B (en) * | 2022-07-12 | 2023-05-09 | 哈尔滨工程大学 | Shark skin-imitated dynamic antifouling material and preparation method thereof |
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Application publication date: 20150826 |