A wear-resistant and weather-resistant organic silicon composite filler and its preparation method and application

Abstract

This invention discloses a wear-resistant and weather-resistant organosilicon composite filler, its preparation method, and application. This invention relates to the technical field of filler preparation. Using nanosilica sol as a seed crystal and a series of organosilicon liquids, such as aluminum sulfate solution and sodium methyl silicate, as raw materials, the filler is prepared through controlled precipitation, washing, drying, and calcination. Application of this filler in epoxy floor paint effectively addresses the wear and weather resistance issues of existing epoxy floor paints. The resulting product is of stable quality, low cost, and simple and efficient operation.

Description

Technical Field

[0001] The present invention relates to the technical field of filler preparation, and in particular to a wear-resistant and weather-resistant organic silicon composite filler, a preparation method thereof, and an application thereof. Background Art

[0002] Epoxy flooring is also known as epoxy resin flooring, epoxy resin flooring, or epoxy flooring. Self-leveling floor paint is a solvent-free, self-leveling, high-build epoxy floor coating with dense particles. In the prior art, epoxy floor paints are generally two-component, one of which often contains a filler, typically talc, quartz powder, mica powder, etc. However, in practice, epoxy floor paints made with such fillers have been found to have poor wear and weather resistance. Summary of the Invention

[0003] The purpose of the present invention is to solve at least one of the technical problems existing in the prior art and to provide a wear-resistant and weather-resistant organic silicon composite filler and a preparation method and application thereof.

[0004] The technical solutions of the present invention are as follows:

[0005] A method for preparing a wear-resistant and weather-resistant organic silicon composite filler comprises the following steps:

[0006] S1: Add nano-silica sol to deionized water at 50-60°C and mix well to prepare a seed solution;

[0007] S2: Pumping aluminum sulfate solution and organic silicate solution into the seed solution in step S1 according to the ratio, adjusting the pH to maintain at 3.0-7.0, and controlling the feed amount to make the solid content of the system 4-5wt% to obtain a mixed slurry;

[0008] S3: The mixed slurry in step S2 is heated to 70-90°C and kept warm for 30-60 minutes to obtain a white slurry; the mixture is then filtered, washed, dried, and crushed in sequence;

[0009] S4: calcining the white powder crushed in step S3 at 600-800° C. for 4-8 hours to obtain an alumina-silicone resin micropowder composite filler.

[0010] Furthermore, in step S1, the organic silicate solution is a mixture of one or more of sodium methyl silicate, potassium methyl silicate, high-boiling sodium silicate, and high-boiling potassium silicate, and its effective solid content is 15-20 wt%.

[0011] Furthermore, in step S1, the seed solution is a dilute silica sol with 0.6-0.85 wt% SiO2.

[0012] Furthermore, in step S2, the mass addition ratio of the aluminum sulfate solution to the silicate solution is 1:8-15.

[0013] Furthermore, in step S2, the concentration of the aluminum sulfate solution is 10-15 wt%.

[0014] Furthermore, in step S2, the pH is adjusted by using a 10-15 wt% hydrochloric acid solution.

[0015] The present invention also discloses a wear-resistant and weather-resistant organic silicon composite filler, which is prepared by any of the above preparation methods.

[0016] The present invention also discloses an application of the wear-resistant and weather-resistant organic silicon composite filler as described above in a coating. Specifically, the coating is composed of component A and component B, wherein component A includes the following components in weight percentage: 65-70% water-based epoxy resin emulsion, 13-18% alumina-silicone resin micropowder composite filler, 0.32-0.37% water-based dispersant, 0.13-0.18% water-based defoamer, 0.22-0.27% water-based leveling agent, 0.23-0.28% surfactant, 8.5-9.5% deionized water, 2-2.5% film-forming aid, and 4.5-5% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:10-15.

[0017] The beneficial effects of the present invention are: the present invention provides a method for preparing a new type of wear-resistant and weather-resistant silicone composite filler, and at the same time, the application of the filler in epoxy floor paint can effectively solve the problem of insufficient wear resistance and weather resistance of existing epoxy floor paint. The product obtained by this method has stable quality, low cost, and a simple and efficient operation process. DETAILED DESCRIPTION

[0018] The following embodiments of the present invention are described in detail. The embodiments described below are exemplary and are only used to explain the present invention, and are not to be construed as limiting the present invention. Where specific techniques or conditions are not specified in the embodiments, the techniques or conditions described in the literature in this field or the product specifications are used. Where the manufacturer of the reagents or instruments is not specified, all are conventional products that can be obtained commercially.

[0019] Example 1:

[0020] S1: Deionized water is pumped into reactor A, stirring is started, the water temperature is controlled at 50-60°C using circulating water, nano-silica sol is added, and after stirring evenly, a seed solution is prepared. The seed solution is a dilute silica sol with 0.6 wt% SiO2;

[0021] S2: Under stirring, a 10wt% aluminum sulfate solution and a 15wt% sodium methyl silicate solution are pumped into the seed solution at the same time according to the ratio. At the same time, 10wt% dilute hydrochloric acid is used as a pH adjuster to maintain the pH at 3. The mass ratio of the aluminum sulfate solution to the sodium methyl silicate solution is 1:8. The feed amount is controlled to make the solid content of the system 4wt%;

[0022] S3: After the feeding is completed, the temperature is raised to 70°C and kept at this temperature for 30 minutes to obtain a white slurry; the obtained slurry is then filtered, collected, washed, and dried using a filter press;

[0023] S4: After drying and crushing, a white powder is obtained, which is further calcined at 600° C. for 4 h to remove bound water, ultimately obtaining a loose and smooth alumina-silicone resin micropowder composite filler.

[0024] S5: An application method of alumina-silicone resin micropowder composite filler, which is composed of component A and component B, wherein component A includes the following components in weight percentage: 65% water-based epoxy resin emulsion, 18% alumina-silicone resin micropowder composite filler, 0.32% water-based dispersant, 0.18% water-based defoaming agent, 0.22% water-based leveling agent, 0.28% surfactant, 9.5% deionized water, 2% film-forming aid, and 4.5% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:15.

[0025] Example 2:

[0026] S1: Deionized water is pumped into reactor A, stirring is started, the water temperature is controlled at 50-60°C using circulating water, nano-silica sol is added, and after stirring evenly, a seed solution is prepared. The seed solution is a dilute silica sol with 0.65 wt% SiO2;

[0027] S2: Under stirring, an 11wt% aluminum sulfate solution, a 16wt% solid content sodium methyl silicate, and a potassium methyl silicate mixed solution (mass ratio of 1:1) are pumped into the seed solution at the same time according to the ratio. At the same time, 11wt% dilute hydrochloric acid is used as a pH regulator to maintain the pH at 3.5. The mass ratio of aluminum sulfate solution: mixed solution is 1:9. The feed amount is controlled to make the solid content of the system 4.25wt%;

[0028] S3: After the feeding is completed, the temperature is raised to 75°C and kept at this temperature for 35 minutes to obtain a white slurry; the obtained slurry is then filtered, collected, washed, and dried using a filter press;

[0029] S4: After drying and crushing, a white powder is obtained, which is further calcined at 650° C. for 5 h to remove bound water, thereby finally obtaining a loose and smooth alumina-silicone resin micropowder composite filler.

[0030] S5: An application method of alumina-silicone resin micropowder composite filler, characterized in that it is composed of component A and component B, wherein component A includes the following components in weight percentage: 66% water-based epoxy resin emulsion, 17% alumina-silicone resin micropowder composite filler, 0.33% water-based dispersant, 0.17% water-based defoaming agent, 0.23% water-based leveling agent, 0.27% surfactant, 9.3% deionized water, 2.1% film-forming aid, and 4.6% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:14.

[0031] Example 3:

[0032] S1: Deionized water was pumped into reactor A, stirring was started, the water temperature was controlled at 50-60°C using circulating water, nano-silica sol was added, and after stirring evenly, a seed solution was prepared. The seed solution was a dilute silica sol with 0.7 wt% SiO2;

[0033] S2: Under stirring, a 12wt% aluminum sulfate solution, a 17wt% high-boiling sodium silicate, and a high-boiling potassium silicate mixed solution (mass ratio of 1:1) are pumped into the seed solution at the same time according to the ratio. At the same time, 12wt% dilute hydrochloric acid is used as a pH regulator to maintain the pH at 4. The mass ratio of aluminum sulfate solution: mixed solution is 1:10. The feed amount is controlled to make the solid content of the system 4.5wt%;

[0034] S3: After the feeding is completed, the temperature is raised to 80°C and kept at this temperature for 40 minutes to obtain a white slurry; the obtained slurry is then filtered, collected, washed, and dried using a filter press;

[0035] S4: After drying and crushing, a white powder is obtained, which is further calcined at 700° C. for 6 h to remove bound water, ultimately obtaining a loose and smooth alumina-silicone resin micropowder composite filler.

[0036] S5: An application method of alumina-silicone resin micropowder composite filler, characterized in that it is composed of component A and component B, wherein component A includes the following components in weight percentage: 67% water-based epoxy resin emulsion, 16% alumina-silicone resin micropowder composite filler, 0.34% water-based dispersant, 0.16% water-based defoaming agent, 0.24% water-based leveling agent, 0.26% surfactant, 9.1% deionized water, 2.2% film-forming aid, and 4.7% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:13.

[0037] Example 4:

[0038] S1: Deionized water was pumped into reactor A, stirring was started, the water temperature was controlled at 50-60°C using circulating water, nano-silica sol was added, and after stirring evenly, a seed solution was prepared. The seed solution was a dilute silica sol with 0.75 wt% SiO2;

[0039] S2: Under stirring, a mixed solution of 13wt% aluminum sulfate solution, 18wt% sodium methyl silicate, and high-boiling sodium silicate (mass ratio of 1:1) is pumped into the seed solution at the same time according to the ratio. At the same time, 13wt% dilute hydrochloric acid is used as a pH regulator to maintain the pH at 5. The mass ratio of aluminum sulfate solution to the mixed solution is 1:12. The feed amount is controlled to make the solid content of the system 4.75wt%;

[0040] S3: After the feeding is completed, the temperature is raised to 85°C and kept at this temperature for 45 minutes to obtain a white slurry; the obtained slurry is then filtered, collected, washed, and dried using a filter press;

[0041] S4: After drying and crushing, a white powder is obtained, which is further calcined at 750° C. for 6.5 h to remove bound water, thereby finally obtaining a loose and smooth alumina-silicone resin micropowder composite filler.

[0042] S5: An application method of alumina-silicone resin micropowder composite filler, characterized in that it is composed of component A and component B, wherein component A includes the following components in weight percentage: 68% water-based epoxy resin emulsion, 15% alumina-silicone resin micropowder composite filler, 0.35% water-based dispersant, 0.15% water-based defoaming agent, 0.25% water-based leveling agent, 0.25% surfactant, 8.5% deionized water, 2.5% film-forming aid, and 5% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:12.

[0043] Example 5:

[0044] S1: Deionized water is pumped into reactor A, stirring is started, the water temperature is controlled at 50-60°C using circulating water, nano-silica sol is added, and after stirring evenly, a seed solution is prepared. The seed solution is a dilute silica sol with 0.8 wt% SiO2;

[0045] S2: Under stirring, a 14wt% aluminum sulfate solution, a 19wt% solid content potassium methyl silicate solution, and a high-boiling potassium silicate (mass ratio of 1:1) mixed solution are pumped into the seed solution simultaneously according to the ratio. At the same time, 14wt% dilute hydrochloric acid is used as a pH regulator to maintain the pH at 6. The mass ratio of the aluminum sulfate solution to the mixed solution is 1:13. The feed amount is controlled to make the solid content of the system 5.0wt%;

[0046] S3: After the feeding is completed, the temperature is raised to 90°C and kept at this temperature for 50 minutes to obtain a white slurry; the obtained slurry is then filtered, collected, washed, and dried using a filter press;

[0047] S4: After drying and crushing, a white powder is obtained, which is further calcined at 800° C. for 7 h to remove bound water, ultimately obtaining a loose and smooth alumina-silicone resin micropowder composite filler.

[0048] S5: An application method of alumina-silicone resin micropowder composite filler, characterized in that it is composed of component A and component B, wherein component A includes the following components in weight percentage: 69% water-based epoxy resin emulsion, 14% alumina-silicone resin micropowder composite filler, 0.36% water-based dispersant, 0.14% water-based defoaming agent, 0.26% water-based leveling agent, 0.24% surfactant, 8.7% deionized water, 2.4% film-forming aid, and 4.9% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:11.

[0049] Example 6:

[0050] S1: Deionized water was pumped into reactor A, stirring was started, the water temperature was controlled at 50-60°C using circulating water, nano-silica sol was added, and after stirring evenly, a seed solution was prepared. The seed solution was a dilute silica sol with 0.85 wt% SiO2;

[0051] S2: Under stirring, a 15wt% aluminum sulfate solution and a 20wt% high-boiling sodium silicate solution are pumped into the seed solution at the same ratio. 15wt% dilute hydrochloric acid is used as a pH adjuster to maintain the pH at 7. The mass ratio of the aluminum sulfate solution to the mixed solution is 1:15. The feed rate is controlled to make the solid content of the system 5.0wt%;

[0052] S3: After the feeding is completed, the temperature is raised to 90°C and kept at this temperature for 60 minutes to obtain a white slurry; the obtained slurry is then filtered, collected, washed, and dried using a filter press;

[0053] S4: After drying and crushing, a white powder is obtained, which is further calcined at 800° C. for 8 h to remove bound water, ultimately obtaining a loose and smooth alumina-silicone resin micropowder composite filler.

[0054] S5: An application method of alumina-silicone resin micropowder composite filler, characterized in that it is composed of component A and component B, wherein component A includes the following components in weight percentage: 70% water-based epoxy resin emulsion, 13% alumina-silicone resin micropowder composite filler, 0.37% water-based dispersant, 0.13% water-based defoaming agent, 0.27% water-based leveling agent, 0.23% surfactant, 8.9% deionized water, 2.3% film-forming aid, and 4.8% cosolvent; wherein component B is an epoxy curing agent; A:B = 100:10.

[0055] Comparative Example 1:

[0056] Compared with Example 1, the difference is that the pH is maintained at 8.0 during feeding.

[0057] Comparative Example 2:

[0058] Compared with Example 1, the difference is that in S2, the feed amount is controlled so that the solid content of the system is 7 wt%.

[0059] Comparative Example 3:

[0060] Compared with Example 1, the difference is that the seed solution in S1 is a dilute silica sol with 0.3 wt% SiO2.

[0061] Comparative Example 4:

[0062] The coating consists of component A and component B, wherein component A includes the following components in weight percentage: 83% water-based epoxy resin emulsion, 0.35% water-based dispersant, 0.15% water-based defoamer, 0.25% water-based leveling agent, 0.25% surfactant, 8.5% deionized water, 2.5% film-forming aid, and 5% cosolvent; component B is an epoxy curing agent; A:B = 100:10.

[0063] The following performance tests were performed on the above embodiments and comparative examples, and the test results are shown in Table 1.

[0064] 1. Wear resistance test

[0065] The loss value of the sample is measured according to GB / T 1768-2006, and the unit is mg.

[0066] 2. Weather resistance test

[0067] The test was carried out according to the ultraviolet lamp test method in GB / T 23987-2009.

[0068] 3. Salt spray resistance

[0069] The test is carried out with reference to the salt spray test of GB / T 1771.

[0070] Table 1 Performance test results of the embodiments and comparative examples

[0071]

[0072]

[0073] The preparation methods of Examples 1 to 6 are roughly the same. Within the range of preparation conditions, soft and fine powders can be prepared by simple grinding.

[0074] The difference between Comparative Example 1 and Example 1 is that the pH of the preparation is relatively high, which will produce gel blocks during the preparation, resulting in coarse particles after drying and grinding. When the coating is made, the particle size is large and the distribution is uneven, resulting in a significant reduction in the density of the coating. Therefore, the wear resistance, weather resistance, and salt spray resistance are all deviated.

[0075] The difference between Comparative Example 2 and Example 1 is that the feed amount is larger, which makes the solid content of the synthesis system higher. At the same seed concentration, the high feed amount causes the particles to grow too large and sandy, and a uniform coarse powder is obtained. When the powder is too coarse, the density of the coating decreases, so the wear resistance, weather resistance, and salt spray resistance are all deviated.

[0076] The difference between Comparative Example 3 and Example 1 is that the initial seed concentration is relatively small. Under the same feed amount, the seed concentration is too small, resulting in the final generated particles being coarse and sandy, which ultimately leads to a decrease in coating density, so the wear resistance, weather resistance, and salt spray resistance are all deviated.

[0077] The above-described embodiments merely represent preferred implementations of the present invention. While the descriptions thereof are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make various other corresponding changes and modifications based on the technical solutions and concepts described above, and all such changes and modifications should fall within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing a wear-resistant and weather-resistant organic silicon composite filler, characterized in that: The following steps are involved: S1: Add nano-silica sol to deionized water at 50-60°C and mix well to prepare a seed solution; S2: adding aluminum sulfate solution and organic silicate solution to the seed solution in step S1 according to the ratio, adjusting the pH to maintain at 3.0-7.0, and controlling the feed amount to make the solid content of the system 4-5wt% to obtain a mixed slurry; S3: The mixed slurry in step S2 is heated to 70-90°C and kept warm for 30-60 minutes to obtain a white slurry; the mixture is then filtered, washed, dried, and crushed in sequence; S4: calcining the white powder crushed in step S3 at 600-800° C. for 4-8 hours to obtain an alumina-silicone resin micropowder composite filler; In step S1, the seed solution is a dilute silica sol with 0.6-0.85 wt% SiO2.

2. The method for preparing a wear-resistant and weather-resistant organic silicon composite filler according to claim 1, characterized in that: In step S1, the organic silicate solution is a mixture of one or more of sodium methyl silicate, potassium methyl silicate, high-boiling sodium silicate, and high-boiling potassium silicate, and its effective solid content is 15-20 wt%.

3. The method for preparing a wear-resistant and weather-resistant organic silicon composite filler according to claim 1, characterized in that: In step S2, the mass addition ratio of the aluminum sulfate solution to the silicate solution is 1:8-15.

4. The method for preparing a wear-resistant and weather-resistant organic silicon composite filler according to claim 1, characterized in that: In step S2, the concentration of the aluminum sulfate solution is 10-15 wt%.

5. The method for preparing a wear-resistant and weather-resistant organic silicon composite filler according to claim 1, characterized in that: In step S2, the pH is adjusted using a 10-15 wt% hydrochloric acid solution.

6. A wear-resistant and weather-resistant organic silicon composite filler, characterized in that: The method is as described in any one of claims 1 to 5.

7. Use of the wear-resistant and weather-resistant organic silicon composite filler according to claim 6 in coatings.

8. A use according to claim 7, characterized in that The coating consists of component A and component B, wherein component A includes the following components in weight percentage: 65-70% water-based epoxy resin emulsion, 13-18% alumina-silicone resin micropowder composite filler, 0.32-0.37% water-based dispersant, 0.13-0.18% water-based defoamer, 0.22-0.27% water-based leveling agent, 0.23-0.28% surfactant, 8.5-9.5% deionized water, 2-2.5% film-forming aid, and 4.5-5% cosolvent; component B is an epoxy curing agent; the ratio of A:B is 100:10-15.

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