Waterproof and fireproof insulating sealant and preparation method thereof

Abstract

The invention discloses a waterproof and fireproof insulating sealant and a preparation method thereof, and belongs to the technical field of sealants. The waterproof and fireproof insulating sealant comprises the following components in parts by weight: 50-80 parts of modified vinyl silicone rubber, 10-30 parts of an inorganic flame retardant, 5-15 parts of an insulating flame-retardant composite material, 2-8 parts of polydisiloxane, 1-5 parts of dimethyl thiourea, 1-5 parts of methyl silicone oil, 1-5 parts of a preservative, 1-5 parts of an additive and 1-2 parts of pigment, the modified vinyl silicone rubber is obtained by modifying vinyl silicone rubber; the insulating flame-retardant composite material is prepared from bisphenol A type epoxy resin, o-hydroxybenzaldehyde and o-aminophenol. The sealant prepared by the method has excellent waterproof, flame-retardant and insulating properties.

Description

Technical Field

[0001] The invention belongs to the technical field of sealants, and in particular relates to a waterproof and fireproof insulating sealant and a preparation method thereof. Background Art

[0002] As modern society's requirements for safety performance continue to increase, the market demand for waterproof and fireproof insulation sealants is growing. In the field of electronics and electrical appliances, this sealant can be used to protect circuit boards, connectors and other sensitive components to improve product safety and reliability. In the construction industry, it can be used to seal windows, door frames and other parts of high-rise buildings to enhance the fire and water resistance of buildings. In the field of transportation, especially in public transportation and commercial vehicles, waterproof and fireproof insulation sealants can improve the safety performance of the vehicle interior and reduce the risk of fire.

[0003] Waterproof and fireproof insulating sealant is a multifunctional special sealing material. It not only provides excellent waterproof performance and prevents water intrusion, but also has good fire retardant performance. It can slow down the spread of fire when a fire occurs, while ensuring electrical insulation performance and preventing current leakage. Therefore, waterproof and fireproof insulating sealant is widely used in many fields such as construction, electronics, ships, aerospace, etc., especially in sealing operations that require high safety standards and harsh environmental conditions. It can provide comprehensive protection and ensure the integrity and safety of the structure. However, the sealant in the prior art does not further improve the waterproof and fireproof insulation performance by modifying and matching the flame retardant component with the matrix component. Summary of the invention

[0004] The purpose of the present invention is to provide a waterproof and fireproof insulating sealant and a preparation method thereof, so as to solve the technical problem that the sealant in the prior art has not further improved the waterproof and fireproof insulating performance by modifying and matching the flame retardant component with the matrix component.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The invention provides a waterproof and fireproof insulating sealant, comprising the following components in parts by weight: 50-80 parts of modified vinyl silicone rubber, 10-30 parts of inorganic flame retardant, 5-15 parts of insulating flame retardant composite material, 2-8 parts of polydisiloxane, 1-5 parts of dimethylthiourea, 1-5 parts of methyl silicone oil, 1-5 parts of preservative, 1-5 parts of additive and 1-2 parts of pigment; the modified vinyl silicone rubber is obtained by modifying vinyl silicone rubber; the insulating flame retardant composite material is prepared from bisphenol A epoxy resin, o-hydroxybenzaldehyde and o-aminophenol.

[0007] Furthermore, the preparation of the modified vinyl silicone rubber comprises the following steps:

[0008] (1) Adding modifier 1: weighing vinyl silicone rubber and placing it in a beaker, adding modifier 1 and stirring, and mixing thoroughly to obtain a modifier-silicone rubber mixture;

[0009] (2) Adding modifier 2: Weigh modifier 2 and add it to the silicone rubber mixture of modifier 1, stir and mix thoroughly to obtain modified vinyl silicone rubber.

[0010] Furthermore, in step (1), the modifier 1 is a mixture of nano-silica and glass fiber, the mass ratio of vinyl silicone rubber to modifier 1 is (50-80):(5-15), and the mass ratio of nano-silica to glass fiber is (2-4):1; in step (2), the modifier 2 is perfluoroalkyltriethoxysilane, and the mass ratio of vinyl silicone rubber to modifier 2 is (50-80):(1-5).

[0011] Furthermore, the preparation of the insulating composite material comprises the following steps:

[0012] Q1, o-hydroxybenzaldehyde, triethylamine and ethyl acetate were added to a three-necked flask connected to a reflux tube, stirred to obtain an ethyl acetate mixture, p-methylphenylphosphoryl dichloride was mixed with ethyl acetate, and dripped into the three-necked flask under nitrogen protection. After the dropwise addition was completed, the reaction temperature was increased, and after the reaction was completed, an intermediate product was obtained;

[0013] Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed with saturated brine, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product;

[0014] Q3, add o-aminophenol and anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the dripping is completed, increase the reaction temperature, and after the reaction is completed, an organic flame retardant is obtained;

[0015] Q4. Weigh the organic flame retardant and bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame retardant composite material.

[0016] In the above process, the synthetic reaction formula involved in the preparation of organic flame retardants is as follows:

[0017]

[0018] After mass spectrometry detection, the mass spectrum results of the intermediate product were: m / z: 380.08 (100.0%), 381.08 (22.7%), 382.09 (3.6%); the mass spectrum results of the organic flame retardant were: m / z: 562.17 (100.0%), 563.17 (36.2%), 564.17 (7.5%).

[0019] Furthermore, in Q1, the molar ratio of o-hydroxybenzaldehyde, p-methylphenylphosphoryl chloride, triethylamine and ethyl acetate is 1:(0.4-0.6):(2.5-3.5):(32-36), the stirring speed is 50-90rpm, the stirring temperature is 20-28°C, and the stirring time is 30-60min; the molar ratio of p-methylphenylphosphoryl chloride to ethyl acetate is 1:(1.3-1.8); the temperature of dripping into the three-necked flask is 0-2°C, the reaction temperature is increased to 60-65°C, and the reaction time is 20-26h; Q2 is washed with saturated brine 2-3 times; in Q3, the molar ratio of o-aminophenol to anhydrous ethanol is 1:(40-45), the temperature is increased to 50-55°C, and the reaction time is 4-6h; in Q4, the mass ratio of organic flame retardant and bisphenol A epoxy resin is (1-5):(80-90).

[0020] The inorganic flame retardant is a mixture of magnesium hydroxide and aluminum hydroxide, and the mass ratio of magnesium hydroxide to aluminum hydroxide is 1:(1-2); the preservative is a mixture of isothiazolinone and benzalkonium chloride, and the mass ratio is 1:1; the additive is a mixture of 2,6-di-tert-butyl-p-cresol and polyethylene glycol, and the mass ratio is 1:1; the pigment is one or more of phthalocyanine blue, phthalocyanine green, red iron oxide, titanium dioxide and mica titanium.

[0021] A method for preparing a waterproof and fireproof insulating sealant comprises the following steps:

[0022] M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a mixing device, stir them evenly at room temperature to obtain a sealant mixture;

[0023] M2: Heat the sealant mixture, and after the reaction is completed, a waterproof and fireproof insulating sealant is obtained.

[0024] Furthermore, the mixing device in M1 is a high-speed disperser, the stirring speed is 50-100 rpm, and the stirring time is 30-60 min; the heating temperature in M2 is 80-140° C., and the reaction time is 1-3 h.

[0025] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0026] 1. The present invention first provides good elasticity, weather resistance and chemical resistance through modified vinyl silicone rubber, while the addition of inorganic flame retardants and insulating flame retardant composite materials significantly improves the flame retardancy and insulation of the material. In addition, the addition of polydisiloxane ensures that the product can be quickly cross-linked under heating conditions to form a stable network structure, improve the mechanical strength and weather resistance of the sealant, the addition of dimethylthiourea enhances the chemical stability and high temperature resistance of the product, the introduction of methyl silicone oil significantly improves the waterproof performance of the sealant, so that it can still maintain a good sealing effect in a humid environment, the mixed use of preservatives isothiazolinone and benzalkonium chloride effectively inhibits the growth of microorganisms and extends the service life of the product, the addition of additives 2,6-di-tert-butyl-p-cresol and polyethylene glycol not only improves the antioxidant properties of the product, but also improves the fluidity and processing properties of the product, the addition of pigments not only improves the appearance, but also improves the anti-corrosion performance of the product, so that the sealant has higher reliability and stability in complex environments.

[0027] 2. The present invention significantly improves the mechanical strength and wear resistance of vinyl silicone rubber by introducing nano-silica and glass fiber. The addition of nano-silica enhances the surface hardness and crack propagation resistance of vinyl silicone rubber, while the addition of glass fiber enhances the tensile strength and tear resistance of the material. The addition of perfluoroalkyltriethoxysilane further enhances the hydrophobicity and corrosion resistance of vinyl silicone rubber, making its application in complex environments more stable and reliable, improving the waterproof performance of the sealant and extending the service life of the product.

[0028] 3. The present invention synthesizes a flame retardant component containing Schiff base by reacting o-hydroxybenzaldehyde with p-methylphenylphosphoryl dichloride for nucleophilic substitution, and then reacting the mixture with o-aminophenol for condensation reaction, and then mixing the mixture with bisphenol A epoxy resin to obtain a composite material with excellent insulation and flame retardant properties. Bisphenol A epoxy resin provides good mechanical properties and insulation, while the reaction product of o-hydroxybenzaldehyde, triethylamine and ethyl acetate enhances the flame retardant properties of the material. The obtained insulating flame retardant composite material not only has good electrical insulation properties, but also can maintain stability at high temperatures, greatly improving the fireproof properties of the sealant. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Embodiment 1:

[0031] This embodiment discloses a preparation method of modified vinyl silicone rubber, comprising the following steps:

[0032] (1) Adding modifier 1: weigh 50 kg of vinyl silicone rubber and put it in a beaker, add 5 kg of nano-silicon dioxide and 2.5 kg of glass fiber, stir and mix thoroughly to obtain a modifier-silicone rubber mixture;

[0033] (2) Adding modifier 2: Weigh 1 kg of perfluoroalkyl triethoxysilane and add it to the modifier 1 silicone rubber mixture, stir and mix thoroughly to obtain modified vinyl silicone rubber.

[0034] This embodiment discloses a preparation method of an insulating composite material, comprising the following steps:

[0035] Q1. Add 15.2 g of o-hydroxybenzaldehyde, 25.2 g of triethylamine and 156 mL of ethyl acetate into a three-necked flask connected to a reflux tube, stir at a speed of 50 rpm, a temperature of 20 ° C, and stir for 30 min to obtain an ethyl acetate mixture. Mix 8.8 g of p-methylphenylphosphoryl dichloride with 65 mL of ethyl acetate, and drop into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 60 ° C. After reacting for 20 hours, an intermediate product is obtained;

[0036] Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed twice with saturated brine, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product;

[0037] Q3, add 10.9g of o-aminophenol and 233mL of anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 50°C, react for 4 hours, and obtain an organic flame retardant;

[0038] Q4. Weigh 10 g of organic flame retardant and 800 g of bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame-retardant composite material.

[0039] The present embodiment discloses a waterproof and fireproof insulating sealant, comprising the following ingredients in parts by weight: 50 kg of modified vinyl silicone rubber, 5 kg of magnesium hydroxide and 5 kg of aluminum hydroxide, 5 kg of insulating flame-retardant composite material, 2 kg of polydisiloxane, 1 kg of dimethylthiourea, 1 kg of methyl silicone oil, 0.5 kg of isothiazolinone, 0.5 kg of benzalkonium chloride, 0.5 kg of 2,6-di-tert-butyl-p-cresol, 0.5 kg of polyethylene glycol and 1 kg of phthalocyanine blue.

[0040] This embodiment also discloses a method for preparing a waterproof and fireproof insulating sealant, comprising the following steps:

[0041] M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a high-speed disperser, stir at room temperature at a speed of 50 rpm for 30 minutes to obtain a sealant mixture;

[0042] M2: Heat the sealant mixture to 80°C and react for 1 hour to obtain a waterproof and fireproof insulating sealant.

[0043] Embodiment 2:

[0044] This embodiment discloses a preparation method of modified vinyl silicone rubber, comprising the following steps:

[0045] (1) Adding modifier 1: weigh 60 kg of vinyl silicone rubber and put it in a beaker, add 8 kg of nano-silicon dioxide and 2 kg of glass fiber, stir and mix thoroughly to obtain a modifier-silicone rubber mixture;

[0046] (2) Adding modifier 2: Weigh 2 kg of perfluoroalkyl triethoxysilane and add it to the modifier 1 silicone rubber mixture, stir and mix thoroughly to obtain modified vinyl silicone rubber.

[0047] This embodiment discloses a preparation method of an insulating composite material, comprising the following steps:

[0048] Q1, 15.2g o-hydroxybenzaldehyde, 26.5g triethylamine and 159mL ethyl acetate were added to a three-necked flask connected to a reflux tube, the stirring speed was 60rpm, the temperature was 22°C, and the stirring was carried out for 40min to obtain an ethyl acetate mixture, 9.5g p-methylphenylphosphoryl dichloride was mixed with 78mL ethyl acetate, and the mixture was dropped into the three-necked flask under nitrogen protection. After the addition was completed, the reaction temperature was increased to 61°C, and the reaction was carried out for 22h to obtain an intermediate product;

[0049] Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed with saturated brine three times, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product;

[0050] Q3, add 10.9g of o-aminophenol and 236mL of anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 52°C, react for 4 hours, and obtain an organic flame retardant;

[0051] Q4. Weigh 20 g of organic flame retardant and 850 g of bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame-retardant composite material.

[0052] The present embodiment discloses a waterproof and fireproof insulating sealant, comprising the following ingredients in parts by weight: 55 kg of modified vinyl silicone rubber, 6 kg of magnesium hydroxide and 6 kg of aluminum hydroxide, 7 kg of insulating flame-retardant composite material, 3 kg of polydisiloxane, 2 kg of dimethylthiourea, 2 kg of methyl silicone oil, 1 kg of isothiazolinone, 1 kg of benzalkonium chloride, 1 kg of 2,6-di-tert-butyl-p-cresol, 1 kg of polyethylene glycol, 0.5 kg of red iron oxide and 0.5 kg of titanium dioxide.

[0053] This embodiment also discloses a method for preparing a waterproof and fireproof insulating sealant, comprising the following steps:

[0054] M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a high-speed disperser, stir at room temperature at a speed of 60 rpm for 40 minutes to obtain a sealant mixture;

[0055] M2: Heat the sealant mixture to 90°C and react for 2 hours to obtain a waterproof and fireproof insulating sealant.

[0056] Embodiment 3:

[0057] This embodiment discloses a preparation method of modified vinyl silicone rubber, comprising the following steps:

[0058] (1) Adding modifier 1: weigh 60 kg of vinyl silicone rubber and put it in a beaker, add 10 kg of nano-silicon dioxide and 2.5 kg of glass fiber, stir and mix thoroughly to obtain a modifier-silicone rubber mixture;

[0059] (2) Adding modifier 2: Weigh 2.5 kg of perfluoroalkyl triethoxysilane and add it to the modifier 1 silicone rubber mixture, stir and mix thoroughly to obtain modified vinyl silicone rubber.

[0060] This embodiment discloses a preparation method of an insulating composite material, comprising the following steps:

[0061] Q1. Add 15.2 g of o-hydroxybenzaldehyde, 29 g of triethylamine and 165 mL of ethyl acetate into a three-necked flask connected to a reflux tube, stir at a speed of 70 rpm, at a temperature of 24 ° C, stir for 35 min to obtain an ethyl acetate mixture, mix 11.5 g of p-methylphenylphosphoryl dichloride with 85 mL of ethyl acetate, and drop into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 63 ° C, react for 23 h, and obtain an intermediate product;

[0062] Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed with saturated brine three times, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product;

[0063] Q3, add 10.9g of o-aminophenol and 240mL of anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 52°C, react for 5h, and obtain an organic flame retardant;

[0064] Q4. Weigh 30 g of organic flame retardant and 860 g of bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame-retardant composite material.

[0065] The present embodiment discloses a waterproof and fireproof insulating sealant, comprising the following ingredients in parts by weight: 65 kg of modified vinyl silicone rubber, 3 kg of magnesium hydroxide and 6 kg of aluminum hydroxide, 8 kg of insulating flame-retardant composite material, 4 kg of polydisiloxane, 4 kg of dimethylthiourea, 4 kg of methyl silicone oil, 1.8 kg of isothiazolinone, 1.8 kg of benzalkonium chloride, 1.7 kg of 2,6-di-tert-butyl-p-cresol, 1.9 kg of polyethylene glycol and 1 kg of red iron oxide.

[0066] This embodiment also discloses a method for preparing a waterproof and fireproof insulating sealant, comprising the following steps:

[0067] M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a high-speed disperser, stir at room temperature at a speed of 80 rpm for 50 minutes to obtain a sealant mixture;

[0068] M2: Heat the sealant mixture to 100°C and react for 2 hours to obtain a waterproof and fireproof insulating sealant.

[0069] Embodiment 4:

[0070] This embodiment discloses a preparation method of modified vinyl silicone rubber, comprising the following steps:

[0071] (1) Adding modifier 1: weigh 80 kg of vinyl silicone rubber and put it in a beaker, add 10 kg of nano-silicon dioxide and 5 kg of glass fiber, stir and mix thoroughly to obtain a modifier-silicone rubber mixture;

[0072] (2) Adding modifier 2: Weigh 5 kg of perfluoroalkyl triethoxysilane and add it to the modifier 1 silicone rubber mixture, stir and mix thoroughly to obtain modified vinyl silicone rubber.

[0073] This embodiment discloses a preparation method of an insulating composite material, comprising the following steps:

[0074] Q1, 15.2g o-hydroxybenzaldehyde, 35.4g triethylamine and 171.5mL ethyl acetate were added to a three-necked flask connected to a reflux tube, the stirring speed was 90rpm, the temperature was 28°C, and the stirring was performed for 60min to obtain an ethyl acetate mixture, 13.3g p-methylphenylphosphoryl dichloride was mixed with 100mL ethyl acetate, and the mixture was dropped into the three-necked flask under nitrogen protection. After the addition was completed, the reaction temperature was increased to 65°C, and the reaction was performed for 26h to obtain an intermediate product;

[0075] Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed with saturated brine 2-3 times, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product;

[0076] Q3, add 10.9g of o-aminophenol and 263mL of anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 55°C, react for 6 hours, and obtain an organic flame retardant;

[0077] Q4. Weigh 50 g of organic flame retardant and 900 g of bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame-retardant composite material.

[0078] The present embodiment discloses a waterproof and fireproof insulating sealant, comprising the following ingredients in parts by weight: 80 kg of modified vinyl silicone rubber, 10 kg of magnesium hydroxide and 5 kg of aluminum hydroxide, 15 kg of insulating flame-retardant composite material, 8 kg of polydisiloxane, 5 kg of dimethylthiourea, 5 kg of methyl silicone oil, 2.5 kg of isothiazolinone, 2.5 kg of benzalkonium chloride, 2.5 kg of 2,6-di-tert-butyl-p-cresol, 2.5 kg of polyethylene glycol and 1 kg of phthalocyanine green.

[0079] This embodiment also discloses a method for preparing a waterproof and fireproof insulating sealant, comprising the following steps:

[0080] M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a high-speed disperser, stir at room temperature at a speed of 100 rpm for 60 minutes to obtain a sealant mixture;

[0081] M2: Heat the sealant mixture to 140°C and, after reacting for 3 hours, obtain a waterproof and fireproof insulating sealant.

[0082] Embodiment 5:

[0083] This embodiment discloses a preparation method of modified vinyl silicone rubber, comprising the following steps:

[0084] (1) Adding modifier 1: weigh 70 kg of vinyl silicone rubber and put it in a beaker, add 9 kg of nano-silicon dioxide and 4.5 kg of glass fiber, stir and mix thoroughly to obtain a modifier-silicone rubber mixture;

[0085] (2) Adding modifier 2: Weigh 4.5 kg of perfluoroalkyl triethoxysilane and add it to the modifier 1 silicone rubber mixture, stir and mix thoroughly to obtain modified vinyl silicone rubber.

[0086] This embodiment discloses a preparation method of an insulating composite material, comprising the following steps:

[0087] Q1, 15.2g o-hydroxybenzaldehyde, 30g triethylamine and 169mL ethyl acetate were added to a three-necked flask connected to a reflux tube, the stirring speed was 80rpm, the temperature was 26°C, and the stirring was performed for 50min to obtain an ethyl acetate mixture, 13g p-methylphenylphosphoryl dichloride was mixed with 95mL ethyl acetate, and the mixture was dropped into the three-necked flask under nitrogen protection. After the addition was completed, the reaction temperature was increased to 64°C, and the reaction was performed for 24h to obtain an intermediate product;

[0088] Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed with saturated brine three times, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product;

[0089] Q3, add 10.9g of o-aminophenol and 250mL of anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the addition is completed, increase the reaction temperature to 54°C, react for 5h, and obtain an organic flame retardant;

[0090] Q4. Weigh 40 g of organic flame retardant and 900 g of bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame-retardant composite material.

[0091] The present embodiment discloses a waterproof and fireproof insulating sealant, comprising the following ingredients in parts by weight: 70 kg of modified vinyl silicone rubber, 9 kg of magnesium hydroxide and 4.5 kg of aluminum hydroxide, 12 kg of insulating flame-retardant composite material, 7 kg of polydisiloxane, 4 kg of dimethylthiourea, 4 kg of methyl silicone oil, 2 kg of isothiazolinone, 2 kg of benzalkonium chloride, 2 kg of 2,6-di-tert-butyl-p-cresol, 2 kg of polyethylene glycol and 1 kg of titanium dioxide.

[0092] This embodiment also discloses a method for preparing a waterproof and fireproof insulating sealant, comprising the following steps:

[0093] M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a high-speed disperser, stir at room temperature at a speed of 90 rpm for 50 minutes to obtain a sealant mixture;

[0094] M2: Heat the sealant mixture to 130°C and react for 3 hours to obtain a waterproof and fireproof insulating sealant.

[0095] Comparative Example 1:

[0096] Comparative Example 1 Compared with Example 4, in the preparation process of the modified vinyl silicone rubber in Comparative Example 1, no perfluoroalkyltriethoxysilane was added, and other conditions remained unchanged.

[0097] Comparative Example 2:

[0098] Comparative Example 2 Compared with Example 4, in the preparation process of the modified vinyl silicone rubber in Comparative Example 2, no nano-silicon dioxide and glass fiber are added, and other conditions remain unchanged.

[0099] Comparative Example 3:

[0100] Compared with Example 4, in Comparative Example 3, during the preparation of the waterproof and fireproof insulating sealant, no insulating flame-retardant composite material is added, and other conditions remain unchanged.

[0101] Comparative Example 4:

[0102] Comparative Example 4 Compared with Example 4, in the preparation process of the waterproof and fireproof insulating sealant in Comparative Example 4, no methyl silicone oil is added, and other conditions remain unchanged.

[0103] Comparative Example 5:

[0104] Compared with Example 4, in Comparative Example 5, no preservative is added during the preparation of the waterproof and fireproof insulating sealant, and other conditions remain unchanged.

[0105] Comparative Example 6:

[0106] Compared with Example 4, in Comparative Example 6, no additives are added during the preparation of the waterproof and fireproof insulating sealant, and other conditions remain unchanged.

[0107] Experimental example

[0108] The samples prepared in Examples 1-5 and Comparative Examples 1-6 were subjected to performance tests. The water vapor transmission rate of the samples was tested according to GB / T 1037-1988. The flame retardancy of the samples was tested by vertical combustion according to GB / T 2408-2008. The dielectric strength of the samples was tested according to GB / T 1408.1-2016. The corrosion resistance of the samples was tested according to GB / T10125-2021. The mass reduction rate was calculated by the mass reduction rate = [(m 前 -m 后 ) / m 前 ]×100%, the elongation at break of the sample was tested according to GB / T 13022-91, and the test results are shown in Table 1:

[0109] Table 1

[0110]

[0111] It can be seen from the test results in Table 1 that the sealant prepared by Examples 1-5 of the present invention has excellent water resistance, flame retardancy, insulation, corrosion resistance and toughness. By comparing Comparative Example 1 with Examples 1-5, it can be seen that the addition of perfluoroalkyl triethoxysilane can effectively improve the flame retardancy, insulation, corrosion resistance and toughness of the sealant; by comparing Comparative Example 2 with Examples 1-5, it can be seen that the addition of nano-silicon dioxide and glass fiber can effectively improve the corrosion resistance of the sealant; by comparing Comparative Example 3 with Examples 1-5, it can be seen that the addition of insulating flame-retardant composite materials can effectively improve the water resistance, flame retardancy, insulation, corrosion resistance and toughness of the sealant; by comparing Comparative Example 4 with Examples 1-5, it can be seen that the addition of methyl silicone oil can effectively improve the water resistance of the sealant; by comparing Comparative Example 5 with Examples 1-5, it can be seen that the addition of preservatives can effectively improve the corrosion resistance and toughness of the sealant; by comparing Comparative Example 6 with Examples 1-5, it can be seen that the addition of additives can effectively improve the toughness of the sealant.

[0112] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

[0113] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A waterproof and fireproof insulating sealant, characterized in that: The invention comprises the following ingredients in parts by weight: 50-80 parts of modified vinyl silicone rubber, 10-30 parts of inorganic flame retardant, 5-15 parts of insulating flame retardant composite material, 2-8 parts of polydisiloxane, 1-5 parts of dimethylthiourea, 1-5 parts of methyl silicone oil, 1-5 parts of preservative, 1-5 parts of additive and 1-2 parts of pigment; the modified vinyl silicone rubber is obtained by modifying vinyl silicone rubber; the insulating flame retardant composite material is prepared from bisphenol A epoxy resin, o-hydroxybenzaldehyde and o-aminophenol.

2. A waterproof and fireproof insulating sealant according to claim 1, characterized in that: The preparation method of modified vinyl silicone rubber comprises the following steps: (1) Weighing vinyl silicone rubber and placing it in a beaker, adding modifier 1 and stirring, and mixing thoroughly to obtain a modifier-silicone rubber mixture; (2) Weighing modifier 2, adding it to the modifier 1 silicone rubber mixture, stirring and mixing thoroughly to obtain modified vinyl silicone rubber.

3. A waterproof and fireproof insulating sealant according to claim 2, characterized in that: In step (1), the modifier 1 is a mixture of nano-silicon dioxide and glass fiber, the mass ratio of vinyl silicone rubber to modifier 1 is (50-80):(5-15), and the mass ratio of nano-silicon dioxide to glass fiber is (2-4):1; in step (2), the modifier 2 is perfluoroalkyltriethoxysilane, and the mass ratio of vinyl silicone rubber to modifier 2 is (50-80):(1-5).

4. The waterproof and fireproof insulating sealant according to claim 1, characterized in that: A method for preparing an insulating composite material comprises the following steps: Q1, o-hydroxybenzaldehyde, triethylamine and ethyl acetate were added to a three-necked flask connected to a reflux tube, stirred to obtain an ethyl acetate mixture, p-methylphenylphosphoryl dichloride was mixed with ethyl acetate, and dripped into the three-necked flask under nitrogen protection. After the dropwise addition was completed, the reaction temperature was increased, and after the reaction was completed, an intermediate product was obtained; Q2, the intermediate product was filtered to remove the white precipitate, the filtrate was washed with saturated brine, and then dried over anhydrous sodium sulfate to obtain a clean intermediate product; Q3, add o-aminophenol and anhydrous ethanol into a three-necked flask connected to a reflux tube, dissolve the clean intermediate product in anhydrous ethanol, and slowly drip it into the three-necked flask under nitrogen protection. After the dripping is completed, increase the reaction temperature, and after the reaction is completed, an organic flame retardant is obtained; Q4. Weigh the organic flame retardant and bisphenol A epoxy resin, mix them evenly, and obtain an insulating flame retardant composite material.

5. A waterproof and fireproof insulating sealant according to claim 4, characterized in that: The molar ratio of o-hydroxybenzaldehyde, p-methylphenylphosphoryl chloride, triethylamine and ethyl acetate in Q1 is 1:(0.4-0.6):(2.5-3.5):(32-36), the stirring speed is 50-90rpm, the stirring temperature is 20-28℃, and the stirring time is 30-60min; the molar ratio of p-methylphenylphosphoryl chloride to ethyl acetate is 1:(1.3-1.8); the temperature of dripping into the three-necked flask is 0-2℃, the reaction temperature is increased to 60-65℃, and the reaction time is 20-26h; Q2 is washed with saturated brine 2-3 times; the molar ratio of o-aminophenol to anhydrous ethanol in Q3 is 1:(40-45), the temperature is increased to 50-55℃, and the reaction time is 4-6h; the mass ratio of organic flame retardant and bisphenol A epoxy resin in Q4 is (1-5):(80-90).

6. The waterproof and fireproof insulating sealant according to claim 1, characterized in that: The inorganic flame retardant is a mixture of magnesium hydroxide and aluminum hydroxide, and the mass ratio of magnesium hydroxide to aluminum hydroxide is 1:(1-2); the preservative is a mixture of isothiazolinone and benzalkonium chloride, and the mass ratio is 1:1; the additive is a mixture of 2,6-di-tert-butyl-p-cresol and polyethylene glycol, and the mass ratio is 1:1; the pigment is one or more of phthalocyanine blue, phthalocyanine green, red iron oxide, titanium dioxide and mica titanium.

7. A method for preparing a waterproof and fireproof insulating sealant, characterized in that: The steps include: M1: Weigh the modified vinyl silicone rubber, inorganic flame retardant, insulating flame retardant composite material, polydisiloxane, dimethylthiourea, methyl silicone oil, preservative, additive and pigment in this order, put them into a mixing device, stir them evenly at room temperature to obtain a sealant mixture; M2: Heat the sealant mixture, and after the reaction is completed, a waterproof and fireproof insulating sealant is obtained.

8. The method for preparing a waterproof and fireproof insulating sealant according to claim 7, characterized in that: The mixing equipment in M1 is a high-speed disperser, the stirring speed is 50-100rpm, and the stirring time is 30-60min; the heating temperature in M2 is 80-140°C, and the reaction time is 1-3h.

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