Method for detecting acid and alkali resistance of silicon-coated aluminum silver powder

Abstract

The invention discloses a method for detecting acid and alkali resistance of silicon-coated aluminum silver powder. The method comprises the following steps: dispersing the silicon-coated aluminum silver powder and a solvent to obtain a mixed solution; adding the mixed solution into water-based resin, and stirring to obtain a to-be-detected sample; uniformly coating a test paper base material with the to-be-detected sample to form a detection film layer, and curing the detection film layer; titrating the detection film layer with acid or alkali, and recording the foaming time of the detection film layer. According to the method for detecting the acid and alkali resistance of the silicon-coated aluminum silver powder, a test paper direct coating method is adopted, the detection time is shortened to be within 30 minutes, the material consumption is reduced, the energy consumption is reduced, the repeatability RSD of a test result is smaller than or equal to 3.2%, and the correlation with an outdoor solarization test result reaches 0.91 or above.

Description

Technical Field

[0001] The present invention relates to the technical field of aluminum silver powder detection, and particularly to a method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder. Background Art

[0002] In the production process of silicon-coated aluminum silver powder, acid and alkali resistance is a key index to measure the product quality, and accurately controlling this property is crucial for the product performance. The currently used detection methods generally include: weighing silicon-coated aluminum silver powder and mixing it with solid acrylic resin powder to obtain a sample; binding with a small binding machine; electrostatic spraying the bound mixed powder; then placing the sprayed workpiece in an environment of 180°C - 210°C for constant temperature baking for 20 - 30 minutes for curing; taking out the workpiece and cooling it for about 20 minutes to restore it to normal temperature; preparing a NaOH solution with a concentration of 9% - 11%; titrating the NaOH solution on the workpiece by titration method and recording the coating failure time, usually the coating failure time is 60 - 180 minutes.

[0003] However, the above detection method has obvious defects: it needs to go through a complete painting process flow, the process is complex, and the detection time is more than 1 hour; the curing time is up to 20 minutes, and high-temperature curing has potential safety hazards and energy waste; the addition of base powder affects the test accuracy; each detection needs to consume 1.2 g of silicon-coated aluminum silver powder and 40 g of acrylic resin powder, the material consumption is large and the cost is high, and the overall detection cycle exceeds 3 hours. Summary of the Invention

[0004] In view of the above deficiencies in the prior art, the present invention provides a method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder, adopting the direct film coating method on test paper, shortening the detection time to within 30 minutes, reducing the material consumption, reducing the energy consumption, and the repeatability RSD of the test results ≤ 3.2%, and the correlation with the outdoor exposure test results reaches more than 0.91.

[0005] To achieve the above object, the embodiments of the present invention adopt the following technical solutions: A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder, comprising the following steps: Disperse the silicon-coated aluminum silver powder in a solvent to obtain a mixed solution; Add the mixed solution to an aqueous resin and stir to obtain a test sample to be detected; Uniformly coat the test sample to be detected on a test paper substrate to form a detection film layer; Cure the test paper substrate forming the detection film layer; Titrate the detection film layer with an acid or a base and record the foaming time of the detection film layer.

[0006] According to one aspect of the present invention, the solvent is water, alcohol or alcohol ether.

[0007] According to one aspect of the present invention, the aqueous resin is one or a combination of acrylic resin, epoxy resin, and polyurethane.

[0008] According to one aspect of the present invention, the mass ratio of the silicon-coated aluminum silver powder to the solvent is 1:(4 - 9).

[0009] According to one aspect of the present invention, the mass ratio of the silicon-coated aluminum silver powder to the aqueous resin is 1:(15 - 28).

[0010] According to one aspect of the present invention, the dispersion of the silicon-coated aluminum silver powder and the solvent includes ultrasonic dispersion for 2 - 4 minutes.

[0011] According to one aspect of the present invention, the stirring of adding the mixed liquid into the aqueous acrylic resin includes magnetic stirring at 800 - 1200 rpm for 12 - 16 minutes.

[0012] According to one aspect of the present invention, the curing includes baking at a temperature of 90°C - 110°C for 2 - 5 minutes.

[0013] According to one aspect of the present invention, the concentration of the acid or base is 8 - 12%.

[0014] According to one aspect of the present invention, the test paper substrate is an alkali-resistant test paper or an acid-resistant test paper.

[0015] Advantages of the implementation of the present invention: By adopting a ratio system of diluting the silicon-coated aluminum silver powder with a solvent and then adding it to the aqueous resin to obtain a test sample to be detected, uniformly coating the test sample to be detected on the test paper substrate to form a detection film layer, and then baking and curing it for a short time, and cooperating with acid or base titration testing to evaluate the acid and alkali resistance of the silicon-coated aluminum silver powder. Compared with the traditional method, the detection time is shortened from more than 120 minutes to within 30 minutes, and the detection efficiency is greatly improved. Moreover, the amount of aluminum silver powder used in a single detection is reduced, the loss of detection materials is reduced, and the material cost is reduced. During the experiment process, the curing temperature is reduced, the energy consumption is reduced, and the safety risk is significantly reduced. At the same time, there is no need for a binding machine and spraying equipment, and the site adaptability is good. It not only simplifies the cumbersome detection steps, reduces the investment in detection equipment funds, but also is easy to operate. The method for detecting the acid and alkali resistance of the silicon-coated aluminum silver powder innovatively adopts the direct film coating method on the test paper, breaks through the traditional process limitations, the repeatability of the test results RSD≤3.2%, and the correlation with the outdoor exposure test results reaches more than 0.91. Description of the Drawings

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required to be used in the embodiments. Obviously, the following described drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained according to these drawings.

[0017] Figure 1 It is a schematic flow chart of the acid and alkali resistance detection method for silicon-coated aluminum silver powder. Specific implementation manners

[0018] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0019] As Figure 1 shown, an acid and alkali resistance detection method for silicon-coated aluminum silver powder includes the following steps: dispersing the silicon-coated aluminum silver powder and a solvent to obtain a mixed solution; adding the mixed solution into a water-based resin and stirring to obtain a sample to be detected; uniformly coating the sample to be detected on a test paper substrate to form a detection film layer on the test paper substrate; curing the test paper with the formed detection film layer; titrating the detection film layer with an acid or a base, observing the change of the detection film layer and recording the time when the detection film layer foams.

[0020] In practical applications, a mixed solution is obtained by dispersing the silicon-coated aluminum silver powder to be detected and a solvent; the mixed solution is added into a water-based resin and stirred to obtain a sample to be detected. After the sample to be detected is uniformly coated on a test paper substrate to form a detection film layer, it is cured by short-time baking. With the acid or base titration test, after the acid or base contacts the detection film layer, it will react with the detection film layer, and the time when the detection film layer starts to foam is observed and recorded. The acid and alkali resistance of the silicon-coated aluminum silver powder to be detected is evaluated by comparing with the foaming time measured by the above method for a standard silicon-coated aluminum silver powder sample. When the foaming time of the silicon-coated aluminum silver powder to be detected is greater than or equal to the foaming time of the standard silicon-coated aluminum silver powder sample, the acid and alkali resistance of the silicon-coated aluminum silver powder to be detected is qualified.

[0021] In practical applications, the solvent can be selected from water, alcohol or alcohol ether. Specifically, deionized water, n-propanol, isopropanol or propylene glycol methyl ether can be selected.

[0022] In practical applications, the water-based resin can be selected from one or a combination of acrylic resin, epoxy resin, polyurethane.

[0023] In practical applications, the mass ratio of the silicon-coated aluminum silver powder to the solvent is 1:(4 - 9). The mass ratio of the silicon-coated aluminum silver powder to the aqueous resin is 1:(15 - 28). Preferably, 0.35 g - 0.65 g of the silicon-coated aluminum silver powder is selected. The silicon-coated aluminum silver powder and the solvent are dispersed to obtain a mixed solution, and then the mixed solution is added to the aqueous resin and stirred to obtain a test sample to be detected. The thickness of the detection film layer formed by coating the test sample on the test paper substrate is generally 25 - 60 μm.

[0024] In practical applications, the silicon-coated aluminum silver powder and the solvent are ultrasonically dispersed for 2 - 4 minutes. Adding the mixed solution to the aqueous resin and stirring includes magnetic stirring at 800 - 1200 rpm for 12 - 16 min.

[0025] In practical applications, the surface of the test paper substrate is smooth and the thickness is between 1 - 2 cm. Preferably, the test paper substrate is selected from acid-resistant test paper or alkali-resistant test paper.

[0026] In practical applications, the curing includes baking at a temperature of 90°C - 110°C for 2 - 5 minutes until the surface of the test paper is dry and non-sticky.

[0027] In practical applications, if the concentration of the acid or alkali is too high, the reaction will be too fast, thus affecting the result observation. If the concentration of the acid or alkali is too low, the detection time will be increased. Preferably, the concentration of the acid or alkali is 8 - 12%. The alkali can be selected as sodium hydroxide, and the acid can be selected as hydrochloric acid.

[0028] Example 1

[0029] A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder includes the following steps: S1. Take 0.35 g of silicon-coated aluminum silver powder and mix it with 2.3 g of deionized water, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixed solution to 8 g of aqueous acrylic resin for mixing, and magnetic stir at 800 - 1200 rpm for 12 - 16 minutes to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali-resistant test paper with a specification of 100 mm × 50 mm, so that the test sample to be detected forms a uniform film on the surface of the standard alkali-resistant test paper to form a detection film layer; S4. Treat the test paper with the formed detection film layer in an oven at 95 - 105°C for 2 - 5 minutes for rapid curing; S5. Titrate the detection film layer with a NaOH solution with a mass concentration of 10%, and record the time when the detection film layer starts to foam as 3 minutes.

[0030] Example 2

[0031] S1. Take 0.65 g of silicon-coated aluminum silver powder, mix it with 3.7 g of deionized water, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixed solution to 12 g of waterborne acrylic resin for mixing, and magnetically stir at 800 - 1200 rpm for 12 - 16 min to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali-resistant test paper with a specification of 100 mm × 50 mm, and make the test sample to be detected form a uniform film on the surface of the standard alkali-resistant test paper to form a detection film layer; S4. Treat the test paper with the formed detection film layer in an oven at 95 - 105 °C for 2 - 5 minutes for rapid curing; S5. Titrate the detection film layer with a NaOH solution with a mass concentration of 11%, and record the time when the detection film layer starts to foam as 8 minutes.

[0032] Example 3

[0033] S1. Take 0.5 g of silicon-coated aluminum silver powder, mix it with 3 g of deionized water, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixed solution to 10 g of waterborne acrylic resin for mixing, and magnetically stir at 800 - 1200 rpm for 12 - 16 min to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali-resistant test paper with a specification of 100 mm × 50 mm, and make the test sample to be detected form a uniform film on the surface of the standard alkali-resistant test paper to form a detection film layer; S4. Treat the test paper with the formed detection film layer in an oven at 95 - 105 °C for 2 - 5 minutes for rapid curing; S5. Titrate the detection film layer with a NaOH solution with a mass concentration of 10%, and record the time when the detection film layer starts to foam as 5 minutes.

[0034] Example 4

[0035] A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder, comprising the following steps: S1. Take 0.35 g of silicon-coated aluminum silver powder and mix it with 2.3 g of propylene glycol methyl ether, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixed solution to 8 g of waterborne acrylic resin for mixing, and magnetically stir at 800 - 1200 rpm for 12 - 16 minutes to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali-resistant test paper with a specification of 100 mm × 50 mm, and make the test sample to be detected form a uniform film on the surface of the standard alkali-resistant test paper to form a detection film layer; S4. Treat the test paper with the detection film layer in an oven at 95 - 105 °C for 2 - 5 minutes for rapid curing; S5. Titrate the detection film layer with a 10% NaOH solution by mass concentration, and record the time when the detection film layer starts to foam as 3 minutes.

[0036] Example 5

[0037] A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder, comprising the following steps: S1. Take 0.35 g of silicon-coated aluminum silver powder and mix it with 2.3 g of n-propanol, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixed solution to 8 g of epoxy resin for mixing, and magnetically stir at 800 - 1200 rpm for 12 - 16 minutes to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali-resistant test paper with a specification of 100 mm × 50 mm, and make the test sample to be detected form a uniform film on the surface of the standard alkali-resistant test paper to form a detection film layer; S4. Treat the test paper with the detection film layer in an oven at 95 - 105 °C for 2 - 5 minutes for rapid curing; S5. Titrate the detection film layer with a 10% NaOH solution by mass concentration, and record the time when the detection film layer starts to foam as 3 minutes.

[0038] Comparative Example 1 The difference from Example 1 is as follows: The curing step is omitted, specifically as follows: S1. Take 0.35 g of silicon-coated aluminum silver powder and mix it with 2.3 g of deionized water, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixed solution to 8 g of waterborne acrylic resin for mixing, and magnetically stir at 800 - 1200 rpm for 12 - 16 minutes to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali-resistant test paper with a specification of 100 mm × 50 mm, and make the test sample to be detected form a uniform film on the surface of the standard alkali-resistant test paper to form a detection film layer; S4. Titrate the detection film layer with a 10% NaOH solution by mass concentration, and record the time when the detection film layer starts to foam as 10 minutes.

[0039] Comparative Example 2 The difference from Example 1 is: The ratio of silicon-coated aluminum silver powder to deionized water is different.

[0040] S1. Take 0.35 g of silicon-coated aluminum silver powder and mix it with 3.6 g of deionized water, and ultrasonically disperse for 2 - 4 minutes to obtain a mixed solution; S2. Add the mixture to 8 g of waterborne acrylic resin and mix. Stir magnetically at 800 - 1200 rpm for 12 - 16 minutes to obtain a test sample to be detected; S3. Uniformly coat the test sample to be detected on a standard alkali - resistant test paper with a specification of 100 mm × 50 mm, and make the test sample to be detected form a uniform film on the surface of the standard alkali - resistant test paper to form a detection film layer; S4. Treat the test paper with the formed detection film layer in an oven at 95 - 105 °C for 2 - 5 minutes for rapid curing; S5. Titrate the detection film layer with a 10% NaOH solution by mass concentration, and record that the time when the detection film layer starts to foam is 5 minutes.

[0041] Repeatability test: Take silicon - coated aluminum silver powder from 3 different production batches, and label the silicon - coated aluminum silver powder from these 3 different production batches as Sample 1, Sample 2, and Sample 3 respectively. Weigh 6 parallel samples from Sample 1, Sample 2, and Sample 3 respectively for acid - and alkali - resistance performance detection. The detection method is the same as that in Example 1, and record the average time when the detection film layer starts to foam for each parallel sample of Sample 1, Sample 2, and Sample 3. At the same time, calculate the RSD value. The results are shown in Table 1.

[0042] Table 1

[0043] As can be seen from Table 1, the repeatability of the test results RSD ≤ 3.2%. It can be seen that the detection method of the present invention has good repeatability during the experiment.

[0044] Correlation test: Use the method of Example 1 and outdoor exposure method to detect 42 samples of silicon - coated aluminum silver powder simultaneously. Take the time when foaming occurs measured by the method of the present invention as the abscissa and the time when foaming occurs measured by the outdoor exposure method as the ordinate for regression analysis, and obtain the correlation coefficient r ≥ 0.91 between the method of the present invention and the results of the outdoor exposure test.

[0045] It can be seen that the method of the present invention can effectively detect the acid - and alkali - resistance performance of silicon - coated aluminum silver powder and significantly shorten the detection cycle.

[0046] Advantages of the implementation of the present invention: By adopting a ratio system in which aluminum silver powder coated with silicon is diluted with a solvent and then added to an aqueous resin, a test sample to be detected is obtained. After the test sample to be detected is evenly coated on a test paper substrate to form a detection film layer, it is baked for a short time, and acid or alkali titration test is used to evaluate the acid and alkali resistance of the aluminum silver powder coated with silicon. Compared with the traditional method, the detection time is shortened from more than 120 minutes to within 30 minutes, and the detection efficiency is greatly improved. Moreover, the amount of aluminum silver powder used in a single detection is reduced, the loss of detection materials is reduced, and the material cost is reduced. During the experimental process, the curing temperature is reduced, the energy consumption is reduced, and the safety risk is significantly reduced. At the same time, there is no need for a binding machine and spraying equipment, and the site adaptability is good. It not only simplifies the cumbersome detection steps, reduces the investment in detection equipment funds, but also has simple operation. The method for detecting the acid and alkali resistance of the aluminum silver powder coated with silicon innovatively adopts the direct film coating method on the test paper, breaks through the traditional process limitations, the repeatability of the test results RSD≤3.2%, and the correlation with the results of the outdoor exposure test is above 0.91.

[0047] As described above, the above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention should be covered by the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims

1. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder, characterized in that, It includes the following steps: Disperse the silicon-coated aluminum silver powder in a solvent to obtain a mixed solution; Add the mixed solution to the water-based resin and stir to obtain a test sample to be detected; Uniformly coat the test sample to be detected on the test paper substrate to form a detection film layer and cure it; Titrate the detection film layer with an acid or a base and record the foaming time of the detection film layer.

2. The acid and alkali resistance detection method of silicon-coated aluminum silver powder according to claim 1, wherein, The mass ratio of the silicon-coated aluminum silver powder to the solvent is 1:(4 - 9).

3. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, The solvent is water, alcohol or alcohol ether.

4. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, The mass ratio of the silicon-coated aluminum silver powder to the water-based resin is 1:(15 - 28).

5. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, The water-based resin is one or a combination of acrylic resin, epoxy resin, polyurethane.

6. The acid and alkali resistance detection method of silicon-coated aluminum silver powder according to claim 1, characterized in that, The dispersion of the silicon-coated aluminum silver powder in the solvent includes ultrasonic dispersion for 2 - 4 minutes.

7. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, Adding the mixed solution to the water-based resin and stirring includes magnetic stirring at 800 - 1200 rpm for 12 - 16 minutes.

8. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, The curing includes baking at a temperature of 90°C - 110°C for 2 - 5 minutes.

9. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, The concentration of the acid or base is 8 - 12%.

10. A method for detecting the acid and alkali resistance of silicon-coated aluminum silver powder according to claim 1, characterized in that, The test paper substrate is an alkali-resistant test paper or an acid-resistant test paper.

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