Glass flake defoaming agent, and preparation method and application thereof

Abstract

The application discloses a glass flake defoaming agent and a preparation method and application thereof. The glass flake defoaming agent comprises the following raw materials: hydrophobic nano-silica, fatty alcohol polyether amide, styrene, epoxy fatty acid methyl ester, polyether modified trisiloxane, sodium stearate and polyacrylonitrile carbon fiber. The preparation method comprises the following steps: mixing the hydrophobic nano-silica and the polyether modified trisiloxane, adding the styrene and stirring under heating; then adding the fatty alcohol ether amide, the epoxy fatty acid methyl ester, the sodium stearate and the polyacrylonitrile carbon fiber, stirring under heating, ultrasonic oscillation, pH adjustment and preparation. The preparation method is simple and easy to implement, the prepared glass flake defoaming agent can penetrate and immerse into a glass flake foam thin layer, increase surface tension, make the foam in the thin layer break, thereby thoroughly eliminating the bubbles in the glass flake, greatly improving the corrosion resistance, service period of the glass flake and the pass rate of electric spark detection of a glass flake finished product.

Description

Technical Field

[0001] This invention relates to the field of glass processing technology, specifically to a glass flake defoamer, its preparation method, and its application. Background Technology

[0002] During the preparation of glass flake coatings, an oxidation-reduction reaction occurs when the accelerator cobalt naphthenate and the curing agent methyl ethyl ketone peroxide are added, generating numerous small air bubbles in a room-temperature curing system. Additionally, the thorough stirring required during glass flake preparation also introduces air bubbles. Furthermore, uneven substrate surfaces during application introduce air bubbles during coating. The presence of these bubbles creates tiny voids in the cured glass flakes, significantly reducing their anti-corrosion effect and service life. Common defoaming methods employ physical methods, such as using a special roller to apply styrene, but these cannot completely eliminate the microbubbles.

[0003] Defoamers are additives used in glass flake putty. They penetrate into the thin foam layer of glass flakes and, due to increased surface tension, cause the foam layer to rupture, thus removing air bubbles from the glass flakes. However, existing defoamers, when blended with glass flake putty, suffer from poor dispersibility and processability, leading to reduced corrosion resistance, shortened service life, and a certain degree of yield in the produced glass flakes. Therefore, a dedicated defoamer for glass flakes that can simultaneously remove air bubbles and improve the yield, corrosion resistance, and service life of the produced glass flakes urgently needs to be developed. Summary of the Invention

[0004] To address the aforementioned technical problems, the present invention aims to provide a glass flake defoamer, its preparation method, and its application, thereby resolving the existing lack of a defoamer specifically for glass flakes.

[0005] The technical solution of the present invention to solve the above-mentioned technical problems is as follows:

[0006] A glass flake defoamer comprises the following raw materials in parts by weight: 13-15 parts hydrophobic nano silica, 8-10 parts fatty alcohol polyether amide, 34-36 parts styrene, 1.5-2.5 parts epoxy fatty acid methyl ester, 10-12 parts polyether modified trisiloxane, 1-3 parts sodium stearate, and 4-6 parts polyacrylonitrile carbon fiber.

[0007] The beneficial effects of this invention are as follows: The main defoamer of this invention is hydrophobic nano-silica, which is the main active ingredient of the glass flake defoamer. The auxiliary defoamers are fatty alcohol polyether amide, polyether-modified trisiloxane, sodium stearate, and polyacrylonitrile carbon fiber. As active ingredients, they play a regulatory role, improving the surface effect of hydrophobic nano-silica and combining with their own defoaming ability to produce a synergistic effect, further improving the defoaming effect. In addition, hydrophobic nano-silica and polyether-modified trisiloxane can be uniformly dispersed in glass flakes after being mixed with glass flake putty, effectively improving the corrosion resistance of glass flakes. Styrene, as the carrier of the glass flake defoamer, acts as a medium, combining with epoxy fatty acid methyl ester as an emulsifier, so that hydrophobic nano-silica, fatty alcohol polyether amide, polyether-modified trisiloxane, sodium stearate, and polyacrylonitrile carbon fiber are dispersed into fine particles in styrene, thereby better dispersing in glass flake putty and significantly improving the defoaming effect.

[0008] Further, the raw materials include the following parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

[0009] The preparation method of the above-mentioned glass flake defoamer includes the following steps:

[0010] (1) Mix hydrophobic nano-silica with polyether-modified trisiloxane, add styrene, and heat and stir.

[0011] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir, then sonicate and adjust the pH value to obtain the product.

[0012] Furthermore, in step (1), the heating and stirring temperature is 120-140℃, the time is 3-5h, and the speed is 800-1200rpm.

[0013] Preferably, in step (1), the heating and stirring temperature is 130°C, the time is 4 hours, and the speed is 1000 rpm.

[0014] Furthermore, in step (2), the heating and stirring temperature is 70-80℃, the time is 3-5h, and the speed is 500-700rpm.

[0015] Preferably, in step (2), the heating and stirring temperature is 75°C, the time is 4 hours, and the speed is 600 rpm.

[0016] Furthermore, in step (2), the temperature of ultrasonic oscillation is 70-80℃, the time is 20-30 min, and the ultrasonic frequency is 80-100 kHz; the pH is adjusted to 6-7.

[0017] Preferably, in step (2), the ultrasonic oscillation temperature is 75°C, the time is 25 min, and the ultrasonic frequency is 90 kHz; the pH is adjusted to 6.5.

[0018] The above-mentioned glass flake defoamer is used in the preparation of glass flakes.

[0019] Furthermore, the preparation method of glass flakes is as follows: glass flake putty and glass flake defoamer are mixed, stirred, allowed to stand, scraped and coated, and then physical defoaming is performed to obtain the glass flakes.

[0020] Furthermore, the amount of glass flake defoamer added is 0.1% to 0.2% of the mass of the glass flake putty.

[0021] Preferably, the amount of glass flake defoamer added is 0.15% of the mass of the glass flake putty.

[0022] Furthermore, the stirring time is 60–90 min at a speed of 300–400 rpm; the settling time is 2–10 min; and physical defoaming is achieved by pressing with a roller.

[0023] Preferably, the stirring time is 75 minutes and the speed is 350 rpm; the settling time is 5 minutes; and physical defoaming is achieved by crushing with a pressure roller.

[0024] The present invention has the following beneficial effects:

[0025] The preparation method of this invention is simple and easy to implement, and can be widely applied. A glass flake defoamer is prepared using hydrophobic nano-silica, fatty alcohol polyether amide, styrene, epoxy fatty acid methyl ester, polyether-modified trisiloxane, sodium stearate, and polyacrylonitrile carbon fiber as raw materials. When applied to the preparation of glass flakes, this defoamer can penetrate into the glass flake foam layer and be evenly distributed in the layer, increasing the surface tension and causing the foam in the layer to break, thereby completely eliminating air bubbles in the glass flakes. This greatly improves the corrosion resistance, service life, and electrical discharge testing pass rate of the prepared glass flakes. Detailed Implementation

[0026] The principles and features of the present invention are described below with reference to embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Unless otherwise specified, specific conditions or manufacturer-recommended conditions should be followed in the embodiments. Reagents or instruments whose manufacturers are not specified are all commercially available products.

[0027] Example 1:

[0028] A glass flake defoamer comprises the following raw materials in parts by weight: 13 parts hydrophobic nano silica, 8 parts fatty alcohol polyether amide, 34 parts styrene, 1.5 parts epoxy fatty acid methyl ester, 10 parts polyether-modified trisiloxane, 1 part sodium stearate, and 4 parts polyacrylonitrile carbon fiber.

[0029] Its preparation method includes the following steps:

[0030] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 120°C for 5 hours at 800 rpm.

[0031] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 70°C for 5 hours at 500 rpm, then sonicate at 70°C for 30 minutes at an ultrasonic frequency of 80 kHz, adjust the pH value to 6.5, and obtain the product.

[0032] Example 2:

[0033] A glass flake defoamer comprises the following raw materials in parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

[0034] Its preparation method includes the following steps:

[0035] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 130°C for 4 hours at 1000 rpm.

[0036] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0037] Example 3:

[0038] A glass flake defoamer comprises the following raw materials in parts by weight: 15 parts hydrophobic nano silica, 10 parts fatty alcohol polyether amide, 36 parts styrene, 2.5 parts epoxy fatty acid methyl ester, 12 parts polyether-modified trisiloxane, 3 parts sodium stearate, and 6 parts polyacrylonitrile carbon fiber.

[0039] Its preparation method includes the following steps:

[0040] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 140°C for 3 hours at 1200 rpm.

[0041] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 80°C for 3 hours at 700 rpm, then sonicate at 80°C for 20 minutes at 100 kHz ultrasonic frequency, adjust the pH value to 6.5, and obtain the product.

[0042] Comparative Example 1:

[0043] A glass flake defoamer comprises the following raw materials in parts by weight: 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

[0044] Its preparation method includes the following steps:

[0045] (1) Add polyether-modified trisiloxane to styrene and heat and stir at 130°C for 4 hours at 1000 rpm.

[0046] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0047] Comparative Example 2:

[0048] A glass flake defoamer comprises the following raw materials in parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

[0049] Its preparation method includes the following steps:

[0050] (1) Add hydrophobic nano-silica to styrene and heat and stir at 130°C for 4 hours at 1000 rpm.

[0051] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0052] Comparative Example 3:

[0053] A glass flake defoamer comprises the following raw materials in parts by weight: 14 parts hydrophobic nano silica, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

[0054] Its preparation method includes the following steps:

[0055] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 130°C for 4 hours at 1000 rpm.

[0056] (2) Add epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0057] Comparative Example 4:

[0058] A glass flake defoamer comprises the following raw materials in parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 11 parts polyether-modified trisiloxane, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

[0059] Its preparation method includes the following steps:

[0060] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 130°C for 4 hours at 1000 rpm.

[0061] (2) Add fatty alcohol ether amide, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0062] Comparative Example 5:

[0063] A glass flake defoamer comprises the following raw materials in parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, and 5 parts polyacrylonitrile carbon fiber.

[0064] Its preparation method includes the following steps:

[0065] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 130°C for 4 hours at 1000 rpm.

[0066] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester and polyacrylonitrile carbon fiber to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0067] Comparative Example 6:

[0068] A glass flake defoamer comprises the following raw materials in parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, and 2 parts sodium stearate.

[0069] Its preparation method includes the following steps:

[0070] (1) Mix hydrophobic nano silica with polyether modified trisiloxane, add styrene, and heat and stir at 130°C for 4 hours at 1000 rpm.

[0071] (2) Add fatty alcohol ether amide, epoxy fatty acid methyl ester and sodium stearate to the product of step (1), heat and stir at 75°C at 600 rpm for 4 h, then sonicate at 75°C at 90 kHz for 25 min, adjust the pH value to 6.5, and obtain the product.

[0072] Experimental example:

[0073] The glass flake defoamers prepared in Examples 1-3 and Comparative Examples 1-6 were tested respectively. The prepared glass flake defoamers were mixed with glass flake putty (Shanghai Fuchen New Materials Co., Ltd., VEGF-2 medium-temperature glass flake putty). The amount of glass flake defoamer added was 0.15% of the mass of glass flake putty. Then, the mixture was stirred at 350 rpm for 75 min, and then allowed to stand for 5 min. After that, it was scraped into a 2 mm thick glass flake precursor, and then physical defoaming was performed by rolling with a pressure roller. After curing, glass flakes were obtained.

[0074] The glass flakes were tested using a 6000V electric spark tester. 50 test points were taken from each glass flake sample. The pass rate was calculated as (pass points / test points) × 100%.

[0075] The prepared glass flakes were immersed in water at 95℃, 1 mol / L hydrochloric acid solution, and 1 mol / L sodium hydroxide solution for 100 h, respectively. The water resistance and acid and alkali corrosion resistance of the glass flakes were characterized by the weight loss rate. The lower the weight loss rate, the better the water resistance and acid and alkali corrosion resistance of the glass flakes. Weight loss rate = 1 - (mass after immersion for 100 h / initial mass) × 100%.

[0076] The experimental results are shown in Table 1 below:

[0077] Table 1 Characterization of performance parameters of glass flakes

[0078] As can be seen from the data in the table above, the glass flakes prepared in this application embodiment are significantly better than the comparative example in terms of pass rate, water resistance, acid resistance and alkali resistance in the electric spark test. On the one hand, the hydrophobic nano-silica in this invention is the main defoamer, while fatty alcohol polyether amide, polyether-modified trisiloxane, sodium stearate, and polyacrylonitrile carbon fiber, as active ingredients, play a regulatory role. By improving the surface effect of the hydrophobic nano-silica, combined with its own defoaming ability, a synergistic effect is produced, further improving the defoaming effect. Styrene, as the carrier of the glass flake defoamer, acts as a medium, combining with epoxy fatty acid methyl ester as an emulsifier, so that the hydrophobic nano-silica, fatty alcohol polyether amide, polyether-modified trisiloxane, sodium stearate, and polyacrylonitrile carbon fiber are dispersed into fine particles in styrene, thus allowing for better dispersion in the glass flake putty, significantly improving the defoaming effect, and thereby increasing the pass rate of glass flakes in the electrical discharge machining (EDM) test. On the other hand, the hydrophobic nano-silica and polyether-modified trisiloxane can also be uniformly dispersed in the glass flakes after being mixed with the glass flake putty, effectively improving the corrosion resistance of the glass flakes, thereby effectively increasing the service life of the produced glass flakes.

[0079] Example 2 is the best implementation of this application. The glass flakes prepared therefrom have a 100% pass rate in the electric spark test and also have excellent resistance to water and acid and alkali corrosion.

[0080] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A glass flake defoamer, characterized in that, The raw materials include the following parts by weight: 13-15 parts hydrophobic nano silica, 8-10 parts fatty alcohol polyether amide, 34-36 parts styrene, 1.5-2.5 parts epoxy fatty acid methyl ester, 10-12 parts polyether modified trisiloxane, 1-3 parts sodium stearate and 4-6 parts polyacrylonitrile carbon fiber.

2. The glass flake defoamer according to claim 1, characterized in that, The raw materials include the following parts by weight: 14 parts hydrophobic nano silica, 9 parts fatty alcohol polyether amide, 35 parts styrene, 2 parts epoxy fatty acid methyl ester, 11 parts polyether-modified trisiloxane, 2 parts sodium stearate, and 5 parts polyacrylonitrile carbon fiber.

3. The method for preparing the glass flake defoamer according to claim 1 or 2, characterized in that, Includes the following steps: (1) Mix hydrophobic nano-silica with polyether-modified trisiloxane, add styrene, and heat and stir; (2) Add fatty alcohol polyether amide, epoxy fatty acid methyl ester, sodium stearate and polyacrylonitrile carbon fiber to the product of step (1), heat and stir, then sonicate and adjust pH to obtain the product.

4. The method for preparing the glass flake defoamer according to claim 3, characterized in that, In step (1), the heating and stirring temperature is 120~140 ℃, the time is 3~5 h, and the speed is 800~1200 rpm.

5. The method for preparing the glass flake defoamer according to claim 3, characterized in that, In step (2), the heating and stirring temperature is 70~80 ℃, the time is 3~5 h, and the speed is 500~700 rpm.

6. The method for preparing the glass flake defoamer according to claim 3, characterized in that, In step (2), the ultrasonic oscillation temperature is 70~80 ℃, the time is 20~30 min, and the ultrasonic frequency is 80~100 kHz; adjust the pH to 6~7.

7. The use of the glass flake defoamer according to claim 1 or 2 in the preparation of glass flakes.

8. The application of the glass flake defoamer according to claim 7 in the preparation of glass flakes, characterized in that, The glass flakes are prepared by mixing glass flake putty with the glass flake defoamer, stirring, letting stand, scraping, and then performing physical defoaming to obtain the glass flakes.

9. The application of the glass flake defoamer according to claim 8 in the preparation of glass flakes, characterized in that, The amount of glass flake defoamer added is 0.1~0.2% of the mass of the glass flake putty.

10. The application of the glass flake defoamer according to claim 8 in the preparation of glass flakes, characterized in that, The stirring time is 60-90 min, and the speed is 300-400 rpm; the settling time is 2-10 min; the physical defoaming is performed by crushing with a pressure roller.

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