A test method for the hydrolysis performance of a hydrolyzable self-polishing antifouling resin
By measuring the weight loss difference of the resin in specific hydrolytic solution and other component liquids, the problems of long test cycles of hydrolytic self-polishing anti-fouling resins and inaccurate detection results are solved, and rapid and accurate hydrolytic performance evaluation is achieved, and R&D efficiency is improved.
Patent Information
- Application Number
- CN202310148881.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-02-22
- Publication Date
- 2025-09-02
- Estimated Expiration
- 2043-02-22
AI Technical Summary
In the prior art, the hydrolytic self-polishing anti-fouling resin has a long test cycle, making it difficult to quickly distinguish samples with similar hydrolysis properties, and the test results are easily disturbed by water-soluble components, so the hydrolysis properties cannot be accurately obtained.
Specific testing steps are used to measure the weight loss of the resin in the resin hydrolysate and other component hydrolysate respectively, calculate the hydrolysis performance through the difference, and use acidic or alkaline buffer solutions to control the pH and temperature to accelerate the hydrolysis process, shorten the test cycle.
It has achieved rapid testing of hydrolysis performance differences, improved R&D efficiency, accurately measured hydrolysis performance, reduced interference from water-soluble substances, and significantly accelerated the screening speed of hydrolytic self-polished anti-fouling resin.
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Figure CN116593348B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of antifouling coatings, in particular to a method for testing the hydrolysis performance of a hydrolyzable self-polishing antifouling resin. Background Art
[0002] Equipment immersed in seawater is highly susceptible to attack by marine organisms such as bacteria, algae, barnacles, and mussels during use. These microorganisms and plants can quickly cover the surface of the equipment, increasing friction and energy consumption on ships, accelerating fouling and corrosion of marine facilities, blocking the mesh of aquaculture cages, leading to the death of aquacultured organisms, and clogging cooling water pipes in power plants, reducing heat exchange efficiency. These issues pose a serious threat to human marine production activities. These issues have also prompted the development of marine antifouling measures, which are now relatively mature. Among them, antifouling coatings are the most effective, economical, and convenient method. With the global ban on organotin antifouling coatings in 2008, Wuxi self-polishing antifouling coatings gradually gained a dominant position and continue to do so today. Hydrolytic self-polishing antifouling coatings are a key category of Wuxi self-polishing antifouling coatings. Their antifouling mechanism utilizes the hydrolysis of antifouling resin film-forming agents under alkaline conditions. This hydrolysis generates a continuous increase in hydrophilic groups, which continuously abrade the antifouling coating surface under the erosion of seawater at a certain velocity, maintaining a fresh, smooth surface and releasing antifouling agents to achieve the desired antifouling effect. Therefore, as the core technology of antifouling coatings, the hydrolysis performance of resin is directly related to the performance of self-polishing antifouling coatings.
[0003] Currently, the hydrolysis performance of hydrolyzable self-polishing antifouling resins can be measured through seawater immersion experiments. Specifically, the hydrolysis performance of different synthesized resins is measured by immersion time-mass loss curves in artificial seawater under a static environment. The prior art publication "Preparation and Performance Study of Zinc / Silicon-Based Acrylate Antifouling Resins" states that the immersion time-mass loss curve test period for the resin coating is 1000 hours, while the publication "Development of Main-Chain Degradable Polyacrylate Silane Self-Polishing Antifouling Coatings" states that the minimum test period for the time-dependent mass loss rate of a novel main-chain degradable polyacrylate silane resin is 50 days. Current methods for testing the hydrolysis performance of hydrolyzable self-polishing antifouling resins have the following problems: 1. The test period is long; 2. It is difficult to quickly distinguish samples with similar hydrolysis performance; and 3. When testing the hydrolysis performance of hydrolyzable self-polishing antifouling resins using prior art methods, the test results are interfered with by other water-soluble components, making it impossible to accurately determine the hydrolysis performance of the hydrolyzable self-polishing antifouling resins. Therefore, providing a new test method for the hydrolysis performance of hydrolyzable self-polishing antifouling resin is of great significance for guiding the research and development of hydrolyzable self-polishing antifouling resin. Summary of the Invention
[0004] In order to solve the problems existing in the above-mentioned prior art, the present application provides a method for quickly determining the hydrolysis performance of hydrolyzable self-polishing antifouling resins. The method adopts specific testing steps, which can quickly test the differences in the hydrolysis performance of hydrolyzable self-polishing antifouling resins with similar hydrolysis performance, shorten the testing cycle, and at the same time, the method can accurately test the hydrolysis performance of hydrolyzable self-polishing antifouling resins, significantly improving the research and development efficiency of hydrolyzable self-polishing antifouling resins.
[0005] The specific technical solutions of the present invention are:
[0006] A method for rapidly determining the hydrolysis performance of a hydrolyzable self-polishing antifouling resin, comprising the following steps:
[0007] (1) Sample preparation: The resin to be tested is coated on a carrier and weighed to prepare the test sample and other component samples;
[0008] (2) Determination of resin weight loss: Place the test sample in the resin hydrolyzate at a constant temperature and soak it. After soaking, wash, dry and weigh it to make a treated test sample.
[0009] (3) Determination of weight loss of other components: Place the other component sample in the hydrolyzate of other components and soak at a constant temperature. After soaking, wash, dry and weigh to prepare the processed other component sample;
[0010] (4) Calculation: Assume that the weight of the test sample is m1, the weight of the treated test sample is m2, the weight of the other component sample is k1, the weight of the treated other component sample is k2, the resin hydrolysis performance is η, and the area of the resin coated on the carrier is S. The formula for the resin hydrolysis performance is as follows: η = [(m1-m2)-(k1-k2)] / S.
[0011] The present application provides a method for rapidly determining the hydrolysis performance of a hydrolyzable self-polishing antifouling resin, which has the following technical effects: 1. Short testing cycle; 2. Rapid detection of differences in the hydrolysis performance of hydrolyzable self-polishing antifouling resins with similar hydrolysis performance, thereby improving research and development efficiency; 3. Accurate detection of the hydrolysis performance of a hydrolyzable self-polishing antifouling resin. This application addresses the problems existing in the prior art by proposing a new method for testing the hydrolysis performance of a hydrolyzable self-polishing antifouling resin. The applicant has found that the results of testing the hydrolyzable self-polishing resin using the prior art are inconsistent with the antifouling performance test results obtained after the resin is used to prepare an antifouling coating. In addition, in artificial seawater, not only the resin itself undergoes hydrolysis, but other water-soluble substances in the resin also dissolve into the hydrolyzate. Testing the hydrolysis performance of the hydrolyzable self-polishing resin is required during the experimental and research and development phase. Therefore, accurate results cannot be obtained using the prior art when testing the hydrolysis performance of the hydrolyzable self-polishing resin.
[0012] In response to the above-mentioned problems, the present application respectively measures the total weight loss of the hydrolyzable self-polishing antifouling resin in the resin hydrolyzate and the weight loss of other resin components of the hydrolyzable self-polishing antifouling resin in the hydrolyzate of other components, and calculates the hydrolysis performance of the hydrolyzable self-polishing antifouling resin by the difference between the two. The hydrolyzable self-polishing antifouling resin can be slowly hydrolyzed under acidic or alkaline conditions and does not hydrolyze in neutral solutions, while other water-soluble substances in the hydrolyzable self-polishing antifouling resin can be dissolved in acidic, alkaline and neutral solutions. Therefore, the present application utilizes the above-mentioned characteristics to design the above-mentioned testing method.
[0013] In addition, in this application, by setting a specific hydrolysis liquid pH and temperature, the hydrolysis rate of the hydrolyzable self-polishing antifouling resin is significantly increased. The difference in hydrolysis performance of hydrolyzable self-polishing antifouling resins with similar hydrolysis performance can be tested on the 8th day of the test, which can accelerate the screening speed of the hydrolyzable self-polishing antifouling resin.
[0014] Preferably, the pH of the resin hydrolyzate in step (2) is 8-9.
[0015] Preferably, the resin hydrolyzate in step (2) is one or more of a boric acid-borax buffer solution, a sodium barbital-hydrochloric acid buffer solution, a tris(hydroxymethyl)aminomethane-hydrochloric acid buffer solution, and a glycine-sodium hydroxide buffer solution; the use of the buffer solution is to keep the pH of the resin hydrolyzate constant, thereby ensuring that the test results are not affected by other environmental factors.
[0016] Preferably, the constant temperature soaking conditions in step (2) are: temperature 30-50°C, soaking time 2-20 days, and the test sample is tilted at 5-15°.
[0017] Preferably, the pH of the hydrolyzate of other components is 6.9-7.1.
[0018] Preferably, the hydrolyzate of other components in step (3) is deionized water.
[0019] Preferably, the carrier in step (1) is a glass plate, one side of the glass plate is a rough surface, and the length of the glass plate is 6-10 cm, the width is 2-4 cm, and the thickness is 0.1-0.2 cm.
[0020] Preferably, the coating step in step (1) is as follows: covering one end of the carrier, coating the resin on the uncovered end, and drying the carrier after coating.
[0021] Preferably, the wet film thickness of the coating is 200-500 μm.
[0022] Preferably, the drying conditions are: first drying at room temperature for 1 to 3 hours, then drying in a forced air drying oven at 40°C for 24 hours, and then drying in a vacuum drying oven at -0.085 MPa and 40°C for 24 hours. The pH of the boric acid-borax buffer solution in step (2) is 8 to 9.
[0023] Compared with the existing technology, this application has the following technical effects:
[0024] (1) The method provided in this application can accurately determine the hydrolysis performance of hydrolyzable self-polishing antifouling resin;
[0025] (2) The method provided in this application can quickly identify the differences in the hydrolysis properties of hydrolyzable self-polishing antifouling resins with similar hydrolysis properties, and the identification efficiency is high;
[0026] (3) The method provided in this application uses a resin hydrolyzate with a specific pH and a hydrolysis temperature, which can significantly improve the hydrolysis performance of the hydrolyzable self-polishing resin. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 It is a line graph of the hydrolysis performance of the hydrolyzable self-polishing antifouling resin of Example 1 and Comparative Example 1 of the present application.
[0028] Figure 2 It is a line graph of the hydrolysis performance of the hydrolyzable self-polishing antifouling resin of Example 2 and Comparative Example 2 of the present application.
[0029] Figure 3 It is a line graph of the hydrolysis performance of the hydrolyzable self-polishing antifouling resin of Example 3 and Comparative Example 3 of the present application.
[0030] Figure 4 It is a line graph of the hydrolysis performance of the hydrolyzable self-polishing antifouling resin of Example 4 and Comparative Example 4 of the present application. DETAILED DESCRIPTION
[0031] The present invention will be further described below with reference to the embodiments.
[0032] Example 1:
[0033] A method for rapidly determining the hydrolysis performance of a hydrolyzable self-polishing antifouling resin comprises the following steps:
[0034] (1) Sample preparation: First, cover one end of the frosted surface of the glass sample (6 cm long, 2 cm wide, 0.1 cm thick) with a 1 cm wide tape, and then use an SZQ four-sided preparation device to coat the remaining part with resin (the resins are self-made low hydrolysis performance hydrolyzable self-polishing antifouling resin samples 1, 2 and 3). The wet film thickness is controlled at 200 μm. After the coating is completed, dry it at room temperature for 1 hour, remove the covering tape, and then put it into a blast drying oven at 40 ° C for 24 hours. After taking it out, put it into a vacuum drying oven at -0.085 MPa and 40 ° C for 24 hours, and finally put it into a silica gel glass desiccator to cool to room temperature for use. Use a marker to number the uncoated end of the sample with antifouling resin on the prepared frosted surface. Use a balance (with a sensitivity of 0.1 mg) to weigh the prepared test sample and other component samples respectively, and record the weight of the test sample and other component samples;
[0035] (2) Determination of resin weight loss: Place the test sample in a container containing glycine-sodium hydroxide buffer solution (pH 9), tilt the sample plate 5° and place it sideways with the numbered end facing up. The hydrolysis solution should not exceed the upper end of the glass plate. Then seal the container and place it in a 45°C constant temperature water bath for hydrolysis. After a certain period of time, take out the sample plate, soak it in deionized water for 5 minutes, and then place it in a forced air drying oven at 40°C for 24 hours. After taking it out, place it in a vacuum drying oven at -0.085MPa and 40°C for 24 hours. Then place it in a silica gel glass desiccator and cool it to room temperature. Use a balance (sensitivity of 0.1mg) to weigh it and make a treated test sample. Record the weight of the treated test sample.
[0036] (3) Determination of weight loss of other components: Place the other component samples in deionized water (pH 7.0) and soak at a constant temperature. After soaking, wash, dry and weigh to prepare the processed other component samples. The constant temperature soaking conditions, washing, drying and weighing conditions are the same as those in step (2);
[0037] (4) Calculation: Assume that the weight of the test sample is m1, the weight of the treated test sample is m2, the weight of the other component sample is k1, the weight of the treated other component sample is k2, the resin hydrolysis performance is η, and the area of the resin coated on the carrier is S. The formula for the resin hydrolysis performance is as follows: η = [(m1-m2)-(k1-k2)] / S; plot the hydrolysis performance of sample 1, sample 2 and sample 3 into a broken line graph. The hydrolysis performance broken line graph is shown in Figure 1 .
[0038] Example 2:
[0039] A method for rapidly determining the hydrolysis performance of a hydrolyzable self-polishing antifouling resin comprises the following steps:
[0040] (1) Sample preparation: First, cover one end of the frosted surface of the glass sample (8 cm long, 3 cm wide, 0.15 cm thick) with a 1.5 cm wide tape, and then use an SZQ four-sided preparation device to coat the remaining part with resin. The wet film thickness of the resin (the resins are self-made hydrolyzable self-polishing antifouling resin samples 4, 5 and 6 with medium hydrolysis performance) is controlled at 350 μm. After the coating is completed, dry it at room temperature for 1 to 3 hours, remove the covering tape, and then put it in a blast drying oven at 40°C for 24 hours. After taking it out, put it in a vacuum drying oven at -0.085 MPa and 40°C for 24 hours, and finally put it in a silica gel glass desiccator to cool to room temperature for use. Use a marker to number the uncoated end of the sample with antifouling resin on the prepared frosted surface. Use a balance (with a sensitivity of 0.1 mg) to weigh the prepared test sample and other component samples, and record the weight of the test sample and other component samples.
[0041] (2) Determination of resin weight loss: Place the test sample in a container containing sodium barbital-hydrochloric acid buffer solution (pH 8.7), tilt the sample plate 10° and place it sideways with the numbered end facing up. The hydrolysis solution should not exceed the upper end of the glass plate. Then seal the container and place it in a 35°C constant temperature water bath for hydrolysis. After a certain period of time, take out the sample plate, soak it in deionized water for 5 minutes, and then place it in a forced air drying oven at 40°C for 24 hours. After taking it out, place it in a vacuum drying oven at -0.085MPa and 40°C for 24 hours. Then place it in a silica gel glass desiccator and cool it to room temperature. Use a balance (sensitivity of 0.1mg) to weigh it and make a treated test sample. Record the weight of the treated test sample.
[0042] (3) Determination of weight loss of other components: Place the other component samples in deionized water (pH 6.9) and soak at a constant temperature. After soaking, wash, dry and weigh to prepare the processed other component samples. The constant temperature soaking conditions, washing, drying and weighing conditions are the same as those in step (2);
[0043] (4) Calculation: Assume that the weight of the test sample is m1, the weight of the treated test sample is m2, the weight of the treated other component sample is m1, the weight of the treated other component sample is m2, the resin hydrolysis performance is η, and the area of the resin coated on the carrier is S. The formula for the resin hydrolysis performance is as follows: η = [(m1-m2)-(k1-k2)] / S; plot the hydrolysis performance of sample 4, sample 5 and sample 6 into a broken line graph. The hydrolysis performance broken line graph is shown in Figure 2 .
[0044] Example 3:
[0045] A method for rapidly determining the hydrolysis performance of a hydrolyzable self-polishing antifouling resin comprises the following steps:
[0046] (1) Sample preparation: First, cover one end of the frosted surface of the glass sample (10 cm long, 4 cm wide, 0.2 cm thick) with a 2 cm wide tape, and then use an SZQ four-sided preparation device to coat the remaining part with resin. The wet film thickness of the resin (the resins are self-made high hydrolysis performance hydrolyzable self-polishing antifouling resin samples 7, 8 and 9) is controlled at 500 μm. After the coating is completed, dry it at room temperature for 3 hours, remove the covering tape, and then put it into a blast drying oven at 40 ° C for 24 hours. After taking it out, put it into a vacuum drying oven at -0.085 MPa and 40 ° C for 24 hours, and finally put it into a silica gel glass desiccator to cool to room temperature for use. Use a marker to number the uncoated end of the sample with antifouling resin on the prepared frosted surface, weigh it with a balance (sensitivity of 0.1 mg) to make a test sample, and record the weight of the test sample;
[0047] (2) Determination of resin weight loss: Place the test sample in a container containing tris(hydroxymethyl)aminomethane-hydrochloric acid buffer solution (pH 8.4), tilt the sample plate 15° and place it sideways, with the numbered end facing upwards, and the hydrolysis solution covering the upper end of the glass plate. Then seal the container and place it in a 30°C constant temperature water bath for hydrolysis. After a certain period of time, take out the sample plate, soak it in deionized water for 5 minutes, and then place it in a forced air drying oven at 40°C for 24 hours. After taking it out, place it in a vacuum drying oven at -0.085MPa and 40°C for 24 hours, then place it in a silica gel glass desiccator and cool it to room temperature. Use a balance (sensitivity of 0.1mg) to weigh it and make a treated test sample, and record the weight of the treated test sample.
[0048] (3) Determination of weight loss of other components: Place the other component samples in deionized water (pH 7.1) and soak at a constant temperature. After soaking, wash, dry and weigh to prepare the processed other component samples. The constant temperature soaking conditions, washing, drying and weighing conditions are the same as those in step (2);
[0049] (4) Calculation: Assume that the weight of the test sample is m1, the weight of the treated test sample is m2, the weight of the other component sample is m1, the weight of the treated other component sample is m2, the resin hydrolysis performance is η, and the area of the resin coated on the carrier is S. The formula for the resin hydrolysis performance is as follows: η = [(m1-m2)-(k1-k2)] / S; the hydrolysis performance of sample 7, sample 8 and sample 9 is plotted as a line graph. The hydrolysis performance line graph is shown in Figure 3 .
[0050] Example 4:
[0051] A method for rapidly determining the hydrolysis performance of a hydrolyzable self-polishing antifouling resin comprises the following steps:
[0052] (1) Sample preparation: First, cover one end of the frosted surface of the glass sample (8 cm long, 3 cm wide, 0.15 cm thick) with a 1.5 cm wide tape, and then use an SZQ four-sided preparation device to coat the remaining part with resin. The wet film thickness of the resin (the resins are homemade hydrolyzed self-polishing antifouling resin samples 10, 11 and 12) is controlled at 350 μm. After the coating is completed, dry it at room temperature for 1 to 3 hours, remove the covering tape, and then put it in a blast drying oven at 40°C for 24 hours. After taking it out, put it in a vacuum drying oven at -0.085 MPa and 40°C for 24 hours, and finally put it in a silica gel glass desiccator to cool to room temperature for use. Use a marker to number the uncoated end of the sample with antifouling resin on the prepared frosted surface, and use a balance (with a sensitivity of 0.1 mg) to weigh them to make test samples and other component samples, and record the weight of the test samples and other component samples;
[0053] (2) Determination of resin weight loss: Place the test sample in a container containing boric acid-borax buffer solution (pH 8.4), tilt the sample plate 10° and place it sideways, with the numbered end facing up, and the hydrolysis solution covering the upper end of the glass plate. Then seal the container and place it in a 40°C constant temperature water bath for hydrolysis. After a certain period of time, take out the sample plate, soak it in deionized water for 5 minutes, and then place it in a forced air drying oven at 40°C for 24 hours. After taking it out, place it in a vacuum drying oven at -0.085MPa and 40°C for 24 hours, then place it in a silica gel glass desiccator and cool it to room temperature. Use a balance (sensitivity of 0.1mg) to weigh it and make a treated test sample, and record the weight of the treated test sample.
[0054] (3) Determination of weight loss of other components: Place the other component samples in deionized water (pH 6.9) and soak at a constant temperature. After soaking, wash, dry and weigh to prepare the processed other component samples. The constant temperature soaking conditions, washing, drying and weighing conditions are the same as those in step (2);
[0055] (4) Calculation: Assume that the weight of the test sample is m1, the weight of the treated test sample is m2, the weight of the treated other component sample is m1, the weight of the treated other component sample is m2, the resin hydrolysis performance is η, and the area of the resin coated on the carrier is S. The formula for the resin hydrolysis performance is as follows: η = [(m1-m2)-(k1-k2)] / S; plot the hydrolysis performance of sample 4, sample 5 and sample 6 into a broken line graph. The hydrolysis performance broken line graph is shown in Figure 4 .
[0056] Comparative Example 1:
[0057] Compared with Example 1, the resin hydrolyzate in Comparative Example 1 is artificial seawater, and the hydrolysis temperature is 25°C; the other conditions are the same as those in Example 1; the hydrolysis performance of Sample 1, Sample 2 and Sample 3 is plotted as a line graph, and the hydrolysis performance line graph is shown in FIG. Figure 1.
[0058] Comparative Example 2:
[0059] Compared with Example 2, the resin hydrolyzate in Comparative Example 2 is artificial seawater, and the hydrolysis temperature is 25°C; the other conditions are the same as those in Example 2; the hydrolysis performance of Samples 4, 5 and 6 is plotted as a line graph, and the hydrolysis performance line graph is shown in FIG. Figure 2 .
[0060] Comparative Example 3:
[0061] Compared with Example 3, the resin hydrolyzate in Comparative Example 3 is artificial seawater, and the hydrolysis temperature is 25°C; the other conditions are the same as those in Example 3; the hydrolysis performance of Samples 7, 8 and 9 is plotted as a line graph, and the hydrolysis performance line graph is shown in FIG. Figure 3 .
[0062] Comparative Example 4:
[0063] Compared with Example 4, the resin hydrolyzate in Comparative Example 4 was artificial seawater, the hydrolysis temperature was 25°C, and no weight loss measurement of other components was performed; the other conditions were the same as those in Example 4; the hydrolysis performance of Samples 10, 11, and 12 was plotted as a line graph, and the hydrolysis performance line graph is shown in FIG. Figure 4 .
[0064] like Figure 1 As shown, Sample 1, Sample 2 and Sample 3 are all homemade low-hydrolysis performance hydrolyzable self-polishing antifouling resins with similar hydrolysis performance. It can be seen from the figure that the hydrolysis performance difference of the resin in Example 1 is very significant on the 8th day of hydrolysis treatment, while there is still no significant difference in Comparative Example 1 on the 16th day of hydrolysis treatment. Compared with Comparative Example 1, on the 8th day, the hydrolysis performance of Sample 1 in Example 1 is improved by 5.5 times, the hydrolysis performance of Sample 2 is improved by 5.3 times, and the hydrolysis performance of Sample 3 is improved by 5.0 times.
[0065] like Figure 2 As shown, Sample 4, Sample 5 and Sample 6 are all homemade medium-hydrolysis performance hydrolyzable self-polishing antifouling resins with similar hydrolysis performance. It can be seen from the figure that the difference in hydrolysis performance of the resin in Example 2 is very significant on the 8th day of hydrolysis treatment, while there is still no significant difference in Comparative Example 2 on the 16th day of hydrolysis treatment. Compared with Comparative Example 2, on the 16th day, the hydrolysis performance of Sample 4 in Example 2 is improved by 2.5 times, the hydrolysis performance of Sample 5 is improved by 2.8 times, and the hydrolysis performance of Sample 6 is improved by 3.0 times.
[0066] like Figure 3As shown in the figure, Sample 7, Sample 8 and Sample 9 are all homemade high-hydrolysis performance hydrolyzable self-polishing antifouling resins with similar hydrolysis performance. It can be seen from the figure that the difference in the hydrolysis performance of the resin in Example 3 is very significant on the 8th day of hydrolysis treatment, while there is still no significant difference in Comparative Example 3 on the 16th day of hydrolysis treatment. Compared with Comparative Example 3, on the 8th day, the hydrolysis performance of Sample 7 is improved by 2.5 times, the hydrolysis performance of Sample 8 is improved by 2.6 times, and the hydrolysis performance of Sample 9 is improved by 2.8 times.
[0067] like Figure 4 As shown, in Example 4, the method provided by the present application was used to test Samples 10, 11, and 12. Compared with Example 4, Comparative Example 4 used artificial seawater as the hydrolysis solution and did not measure the weight loss of other components. From the results of the hydrolysis rate, it can be seen that the method provided by the present application can be used to obtain the hydrolysis weight loss of sample 12>sample 11>sample 10 at the beginning of hydrolysis for 0-16 days; while using the artificial seawater of Comparative Example 4, the hydrolysis weight loss can be obtained within 0-4 days of hydrolysis as sample 12>sample 10>sample 11, and on the 4th to 16th day of hydrolysis, the hydrolysis weight loss is sample 10>sample 12>sample 11; from the above results, it can be seen that the method provided by the present application can accurately obtain the hydrolysis situation of the hydrolyzable self-polishing resin, can more clearly and accurately grasp the hydrolysis trend of the hydrolyzable self-polishing resin, and is more conducive to guiding the synthesis and screening of the hydrolyzable self-polishing resin during the experimental research and development process.
[0068] In summary, the method provided in this application can accelerate the hydrolysis performance of hydrolyzable self-polishing antifouling resins, can quickly identify the differences in hydrolysis performance of hydrolyzable self-polishing resins with similar hydrolysis performance, and can more clearly and accurately test the hydrolysis trend of acrylic resins in hydrolyzable self-polishing resins, which can significantly improve R&D efficiency.
[0069] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent transformation made to the above embodiment based on the technical essence of the present invention still fall within the scope of protection of the technical solution of the present invention.
Claims
1. A method for testing the hydrolysis performance of a hydrolyzable self-polishing antifouling resin, characterized in that: The following steps are involved: (1) Sample preparation: The resin to be tested is coated on a carrier and weighed to prepare the test sample and other component samples; (2) Determination of resin weight loss: The test sample is placed in a resin hydrolyzate and immersed at a constant temperature. After immersion, it is washed, dried, and weighed to prepare a treated test sample; the resin hydrolyzate includes one or more of boric acid-borax buffer solution, sodium barbital-hydrochloric acid buffer solution, tris(hydroxymethyl)aminomethane-hydrochloric acid buffer solution, and glycine-sodium hydroxide buffer solution; the pH of the resin hydrolyzate is 8-9, and the constant temperature immersion temperature is 30-50°C; (3) Determination of weight loss of other components: Place the sample of other components in the hydrolyzate of other components and soak it at a constant temperature. The pH of the hydrolyzate of other components is 6.9~7.
1. The hydrolyzate of other components is deionized water. After soaking, wash, dry and weigh to prepare the sample of processed other components. The constant temperature soaking conditions, washing, drying and weighing conditions are the same as those in step (2); (4) Calculation: Assume that the weight of the test sample is m1, the weight of the treated test sample is m2, the weight of the other component sample is k1, the weight of the treated other component sample is k2, the resin hydrolysis performance is η, and the area of the resin coated on the carrier is S. The formula for the resin hydrolysis performance is as follows: η = [(m1-m2)-(k1-k2)] / S.
2. The testing method according to claim 1, wherein: The constant temperature soaking condition in step (2) is: the soaking time is 2 to 20 days, and the test sample is placed at an inclination of 5 to 15 degrees.
3. The testing method according to claim 1, wherein: The carrier in step (1) is a glass plate, and one side of the glass plate is a rough surface.
4. The testing method according to claim 3, wherein: The length of the glass plate is 6 to 10 cm.
5. The testing method according to claim 3, wherein: The width of the glass plate is 2 to 4 cm.
6. The testing method according to claim 3, wherein: The thickness of the glass plate is 0.1-0.2 cm.
7. The testing method according to claim 1, wherein: The coating step in step (1) is as follows: covering one end of the carrier, coating the resin on the uncovered end, and drying the carrier after coating.
8. The testing method according to claim 7, wherein: The wet film thickness of the coating is 200-500 μm.
9. The testing method according to claim 7, wherein: The drying conditions are as follows: first drying at room temperature for 1-3 hours, then drying in a forced air drying oven at 40°C for 24 hours, and then drying in a vacuum drying oven at -0.085 MPa and 40°C for 24 hours.