CN111855564A - Method for improving evaluation efficiency of adhesion performance of mussel-resistant material - Google Patents
Method for improving evaluation efficiency of adhesion performance of mussel-resistant material Download PDFInfo
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Abstract
The invention discloses a method for improving the evaluation efficiency of the adhesion performance of a mussel-resistant material, which realizes the simulation of the adhesion process of the mussel by the self-polymerization process of dopamine hydrochloride on the surface of the material; the polydopamine is deposited on the surface of the material to the maximum extent by regulating and controlling the self-polymerization reaction condition of the dopamine hydrochloride; the dopamine hydrochloride self-polymerization reaction conditions are as follows: the pH value of the alkaline solution is 8.5-10; the concentration of the dopamine hydrochloride is 15-21 mmol/L; the concentration of the deposition accelerator is 50-200 mmol/L; the concentration of the deposition regulator is 20-100 mmol/L; the reaction time is 168-240 h; the reaction temperature is 20-30 ℃; cleaning the sample after deposition; the amount of mussel fouling was evaluated using the amount of polydopamine film deposited. The method has the advantages that complicated microbial culture is not needed in the evaluation process, simplicity and convenience are realized, the evaluation result can be quantized, the evaluation efficiency can be obviously improved compared with a real sea hanging method, and the method is suitable for evaluating the anti-mussel adhesion performance of metal and non-metal materials.
Description
Technical Field
The invention belongs to the field of corrosivity, relates to a corrosion and biofouling test method, and particularly relates to a method for evaluating the anti-mussel adhesion performance of a material.
Background
The service process of the material in water environment is inevitably confronted with pollution and microbial corrosion. Taking a seawater environment as an example, within seconds after the material is immersed in seawater, organic macromolecules, organic debris and inorganic matters are adsorbed on the surface of the material, then a large number of bacteria are attached within minutes, and microorganisms such as diatom and the like begin to attach within days; large fouling organisms will attach in the following days to months, most commonly mussels and barnacles. The attachment of large fouling organisms causes a series of problems of ship resistance increase, marine structure dead weight increase, corrosion failure, pipeline blockage and the like. The evaluation of the anti-mussel adhesion performance of the material is a necessary work for developing new antifouling materials and new technology.
As mentioned previously, mussels are one of the major fouling organism species. At present, some methods exist for evaluating the adhesion performance of large fouling organisms such as mussels on the surface of a material, but a plurality of defects still exist.
The China national standard GB/T7789 'dynamic test method for antifouling performance of ship antifouling paint', which is a test plate of antifouling paint is arranged on a rotor test device and continuously operates in natural seawater according to a certain period, so that the sailing state of a ship is simulated. Similarly, the american society for testing and materials standard ASTM D3623 "test method for antifouling panels in shallow immersion" specifies the shallow sea cladding evaluation method for the antifouling performance of low surface energy coatings. Firstly, classifying and marking substances adsorbed to the surface of a coating, such as organic substances, inorganic substances and fine crushed stones; lower algae and diatoms are labeled as one class; the larvae of biofouling organisms were scored as initial fouling; and when large fouling organisms such as barnacles, mussels and oysters appear on the surface, the attachment area of the large fouling organisms is considered. The antifouling property evaluation formula is as follows: FR-1-a-B; wherein FR is antifouling performance, A is the ratio of the attachment area of large fouling organisms to the whole sample area; if the surface of the sample has the fouling organism larvae, recording B as 0.05, otherwise, recording B as 0; the larger the FR value, the better the antifouling property. The method can objectively reflect the antifouling performance of the material in the hang plate sea area, including the adhesion performance of large fouling organisms, but the test period is long, the repeatability is poor, and the requirement of a large amount of screening tests on the effect evaluation in the development stage of the antifouling material cannot be met.
In view of the defects of the actual marine environment hanging plate evaluation method, a laboratory evaluation method is concerned, and patent CN 102023130A discloses a flow channel type marine organism adhesion force testing device, which utilizes a rectangular testing cavity with a large aspect ratio to form a stably developed turbulent flow on the surface of a test sample, utilizes a pressure difference sensor to test the pressure difference of different sites on the surface of the sample, and obtains the adhesion force data of fouling organisms on the surface of a material by calculation. The device consists of a water circulation system and an automatic control system, wherein the water circulation system comprises a settling chamber, a test cavity, a light source and a water tank; the automatic control system comprises a differential pressure transmitter, a variable frequency pump, a flowmeter, a pressure transmitter, a programmable controller and a computer. When the test is carried out, firstly, fouling organisms are collected and cultured in the sea area, then the fouling organisms are attached to the surface of the sample, and then the sample with the fouling organisms attached is placed into a test device for testing. The method realizes the automatic and quantitative evaluation of the fouling condition, but still needs to perform complicated biological culture, has a complex device structure and low evaluation efficiency. The research result of mussel adhesion mechanism shows that the adhesion protein (Mefps) secreted by mussels is a material base capable of firmly attaching to the surface of an object, the hydrolyzed amino acid segment of the adhesion protein (Mefps) contains a large amount of DOPA (DOPA) residues, and the adhesion performance of the Mefps containing the DOPA adhesion protein is enhanced along with the increase of the DOPA content. This indicates that DOPA can be used for biomimetic simulation of mussel adhesion, however, existing studies have focused on modifying the polymer chain segment with DOPA-like substances to obtain biomimetic adhesive materials. Related researches or patents for improving the evaluation efficiency of the anti-mussel adhesion performance of the material by using DOPA substances are not reported yet.
Disclosure of Invention
The invention aims to provide a method for improving the efficiency of evaluating the adhesion performance of a mussel-resistant material, aiming at the defects of the existing method, and the method is suitable for evaluating the adhesion performance of the mussel-resistant material of metal and non-metal materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for improving the efficiency of evaluating the adhesion performance of a material to mussels is characterized in that the simulation of the adhesion process of the mussels is realized by the self-polymerization process of dopamine hydrochloride on the surface of the material; the polydopamine is deposited on the surface of the material to the maximum extent by regulating and controlling the self-polymerization reaction condition of the dopamine hydrochloride. The dopamine hydrochloride self-polymerization reaction conditions are as follows: an alkaline solution (pH 8.5-10); the concentration of the dopamine hydrochloride is 15-21 mmol/L; the concentration of the deposition accelerator is 50-200 mmol/L; the concentration of the deposition regulator is 20-100 mmol/L; the reaction time is 168-240 h; the reaction temperature is 20-30 ℃. Cleaning the sample after deposition; the mussel fouling amount was evaluated using the deposition amount of the polydopamine film, which was calculated by the following formula:
wherein: z is the amount deposited (mg/cm)2)；wnIs the sample weight (mg) after autopolymerization; w is a0Weight of sample before self-polymerization (mg); s is the sample surface area (cm) 2). The smaller the deposition amount, the better the mussel fouling resistance of the tested sample, and the worse the mussel fouling resistance of the tested sample.
The dopamine hydrochloride autopolymerization reaction conditions comprise alkaline solution, pH value, dopamine hydrochloride concentration, deposition promoter concentration, deposition regulator concentration, reaction time and reaction temperature.
The alkaline solution is one of a tris (hydroxymethyl) aminomethane aqueous solution, a NaOH aqueous solution and ammonia water. The dopamine hydrochloride can undergo self-polymerization reaction under the alkaline aerobic condition to generate poly-dopamine which is deposited on the surface of the material. The pH value is too low, and the self-polymerization reaction rate is too slow. Too high a pH value is not favorable for uniform distribution of polydopamine. The concentration of the tris (hydroxymethyl) aminomethane aqueous solution is 10mmol/L, and the concentration of the NaOH aqueous solution is 0.1 mmol/L; the concentration of ammonia water is 0.5 mmol/L; the pH value of the solution is adjusted to 8.5-10 by adopting HCl or NaOH.
The concentration of the dopamine hydrochloride has an important influence on the self-polymerization reaction process. When the concentration of dopamine hydrochloride is too low, the number of monomers participating in self-polymerization reaction is small, and the integrity and the deposition rate of a deposited film are influenced; when the concentration of the dopamine hydrochloride is too high, the self-polymerization reaction is too fast, which is not beneficial to the uniform nucleation of the polydopamine on the surface of the material, and further influences the uniformity of the polydopamine film. The self-polymerization reaction can be carried out under the alkaline aerobic condition, and the reaction is very similar to the adhesion process of the mussel adhesive protein on the surface of the material. The catechol group of dopamine hydrochloride is easily oxidized in oxygen-containing aqueous solution to generate a dopamine quinone compound with a catechol structure. Both dopamine and dopamine quinone can undergo an anti-disproportionation reaction to generate semiquinone free radicals, which are then coupled to form cross-links, thereby forming nuclei for 'growth' on the surface of the material.
The accelerant provides oxidizing substances in the dopamine hydrochloride self-polymerization process, and promotes the deposition of polydopamine on the surface of the material. The concentration of the accelerant is too low, and the deposition rate of polydopamine is slow; too high concentration of accelerator results in too rapid autopolymerization, resulting in poor uniformity of polydopamine film. The promoter is at least one of ammonium persulfate and hydrogen peroxide.
The deposition regulator can inhibit the dopamine hydrochloride from self-polymerizing reaction from being performed too fast, so that the polydopamine film deposited on the surface of the material is more uniform. The deposition regulator is one or more of ethanol, sodium phosphate and sodium dihydrogen phosphate.
The reaction time is an important factor influencing the deposition amount of the polydopamine film layer on the surface of the material and the microscopic morphology of the polydopamine film layer. The reaction time is too short, and a complete and continuous polydopamine film layer cannot be formed on the surface of the material; the reaction time is too long, the deposition amount of polydopamine on the surface of the material is not increased continuously, and the evaluation efficiency is reduced.
The reaction temperature is also a main influence factor of dopamine hydrochloride autopolymerization. The proper reaction temperature can make the polydopamine particles tend to be fine and more uniformly attached to the surface of a sample. The reaction temperature is too low, the polydopamine deposition rate is low, and the deposition amount is small; the reaction temperature is too high, which tends to cause fluctuations in solution concentration due to evaporation and increases the corrosion risk of the metal specimen.
The invention has the beneficial effects that: according to the method for improving the evaluation efficiency of the adhesion performance of the mussel-resistant material, the evaluation process does not need to carry out complicated microbial culture, the method is simple and easy to implement, and the evaluation result can be quantized; compared with the actual sea hanging slice method, the evaluation efficiency can be obviously improved. The method is suitable for evaluating the anti-mussel adhesion performance of metal and non-metal materials.
Detailed Description
The embodiment and the comparative example of the method for improving the efficiency of evaluating the anti-mussel adhesive property of the material are shown in the table 1. The materials used in examples 1 to 9 and comparative example were AH32 made of marine steel, and the material used in example 10 was polytetrafluoroethylene. The specific effects of the examples and comparative examples are shown in Table 2.
TABLE 1 examples of the present invention and comparative examples
TABLE 2 effects of examples and comparative examples
Remarking: the deposited layer has uniform color and uniform film thickness distribution; the delta-deposition layer has more uniform color and luster and more uniform film thickness distribution;
x-uneven color of the deposit and uneven film thickness distribution.
The implementation effect of each embodiment shows that the polydopamine film deposited under the dopamine hydrochloride autopolymerization reaction regulation condition according to the technical scheme of the invention has uniform micro-appearance color and uniform film thickness distribution; the reaction time is 168-240 h, and compared with the method that the adhesion performance of the mussel is evaluated by adopting a real sea hanging piece method, the method takes several months to one year or several years, and the evaluation efficiency of the adhesion performance of the mussel is remarkably improved. The polytetrafluoroethylene used in example 10 is a low-surface energy material, so that the deposition amount and deposition rate of polydopamine on the surface are lower than those of AH32 steel. In comparative example 1, the concentration of dopamine hydrochloride is too low, which is not beneficial to forming a complete polydopamine film, so that the color and luster of the deposited film and the distribution of the film thickness are not uniform; in comparative example 2, no deposition promoter was used, so the deposition amount and deposition rate were significantly lower than those of examples 1-9; in comparative example 3, no deposition regulator was used, resulting in uneven color and luster of the deposited film and uneven distribution of film thickness; in comparative example 4, the reaction time is too short, so that the deposition amount and the deposition rate are significantly lower than those of examples 1 to 9, and the color and the film thickness distribution of the deposited film are not uniform; in comparative example 5, the pH of the alkaline solution was too high, resulting in uneven color and luster of the deposited film and uneven distribution of the film thickness.
The present invention has been described in terms of the above embodiments, and equivalents thereof based on the principles of the invention are not excluded from the scope of the invention.
Claims (5)
1. A method for improving the efficiency of evaluating the adhesion performance of a material to mussels is characterized in that the simulation of the adhesion process of the mussels is realized by the self-polymerization process of dopamine hydrochloride on the surface of the material; the polydopamine is deposited on the surface of the material to the maximum extent by regulating and controlling the self-polymerization reaction condition of the dopamine hydrochloride; the dopamine hydrochloride self-polymerization reaction conditions are as follows: the pH value of the alkaline solution is 8.5-10; the concentration of the dopamine hydrochloride is 15-21 mmol/L; the concentration of the deposition accelerator is 50-200 mmol/L; the concentration of the deposition regulator is 20-100 mmol/L; the reaction time is 168-240 h; the reaction temperature is 20-30 ℃; cleaning the sample after deposition; the mussel fouling amount was evaluated using the deposition amount of the polydopamine film, which was calculated by the following formula:
wherein: z is the amount deposited, mg/cm2；wnIs the sample weight after autopolymerization, mg; w is a0Sample weight before autopolymerization, mg; s is the sample surface area, cm2(ii) a The smaller the deposition amount, the better the mussel fouling resistance of the tested sample, and the worse the mussel fouling resistance of the tested sample.
2. The method for improving the efficiency of evaluating the adhesion of a material to a mussel according to claim 1, wherein the alkaline solution is one of a tris aqueous solution, a NaOH aqueous solution and an ammonia solution, and the pH of the solutions is adjusted to 8.5-10 by HCl or NaOH.
3. The method for improving the efficiency of evaluating the adhesion performance of the material to the mussel, according to claim 2, wherein the concentration of the aqueous solution of tris is 10mmol/L, the concentration of the aqueous solution of NaOH is 0.1 mmol/L; the concentration of ammonia water was 0.5 mmol/L.
4. The method for improving the efficiency of evaluating the adhesion performance of a material to mussel according to claim 1, wherein the deposition promoter is at least one of ammonium persulfate and hydrogen peroxide.
5. The method for improving the efficiency of evaluating the adhesion property of the material to the mussel, according to claim 1, wherein the deposition regulator is one or more of ethanol, sodium phosphate and sodium dihydrogen phosphate.
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| CN110426324A (en) * | 2019-08-27 | 2019-11-08 | 南京大学 | A kind of measuring method of the sub- surface hydrophobicity migration of polyolefin insulation |
| CN110726804A (en) * | 2019-07-11 | 2020-01-24 | 浙江省海洋开发研究院 | Quick evaluation method for antifouling performance of bionic and low-surface-energy marine antifouling coating |
| CN111004391A (en) * | 2019-11-21 | 2020-04-14 | 浙江大学 | Preparation method of size-controllable nano poly dopamine |
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- 2020-07-07 CN CN202010644551.7A patent/CN111855564B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2008070298A (en) * | 2006-09-15 | 2008-03-27 | Tokyo Electric Power Co Inc:The | Corrosion resistance testing method and evaluating method for steel material |
| CN102435604A (en) * | 2011-09-01 | 2012-05-02 | 中国船舶重工集团公司第七二五研究所 | Indoor evaluation method for antifouling properties of foul-release antifouling coatings |
| CN109900628A (en) * | 2019-02-20 | 2019-06-18 | 河海大学 | A kind of experimental provision and corrosion evaluation method of simulating ocean environment corrosion |
| CN110726804A (en) * | 2019-07-11 | 2020-01-24 | 浙江省海洋开发研究院 | Quick evaluation method for antifouling performance of bionic and low-surface-energy marine antifouling coating |
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| CN111004391A (en) * | 2019-11-21 | 2020-04-14 | 浙江大学 | Preparation method of size-controllable nano poly dopamine |
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