Fiber-reinforced fireproof silica gel composite foam and preparation method thereof

Abstract

The invention discloses fiber-reinforced fireproof silica gel composite foam and a preparation method thereof, the foam is obtained by mixing a component A and a component B according to a mass ratio of (0.5-2): (0.5-2), coating, foaming and curing, and the component A comprises the following raw materials: vinyl silicone oil, a platinum catalyst, a powder filler and hydroxyl silicone oil; the component B is prepared from the following raw materials: vinyl silicone oil, hydrogen-containing silicone oil, an inhibitor, ceramic powder and fiber-reinforced base rubber. The chopped fibers are pretreated to prepare the modified fiber pulp, then the modified fiber pulp is mixed with the silica gel, the fireproof silica gel foam is prepared through foaming vulcanization, through the synergistic effect of the modified fiber pulp and ceramic powder in the silica gel foam, the fireproof performance of the foam is enhanced, and meanwhile the rebound resilience of the silica gel foam in the normal temperature state is reserved; according to the invention, by adding the fiber material into the silica gel foam, the foam not only has mechanical properties at normal temperature, but also has fire-resistant and fire-insulating properties at high temperature.

Description

Technical Field

[0001] The invention relates to the field of foam materials, and in particular to a fiber-reinforced fireproof silica gel composite foam and a preparation method thereof. Background Art

[0002] Silicone foam is a necessary material for new energy vehicles and energy storage industries due to its excellent aging performance and weather resistance. With the continuous development of the industry, the safety performance requirements of materials are also gradually increasing. In order to make silicone foam have good fire resistance, inorganic powders such as alumina, magnesium hydroxide, ceramic micropowder and other fireproof fillers are usually added to silicone foam to increase its flame retardancy and fire resistance. Different types of refractory fillers have different performances at ultra-high temperatures (≥800C). Inorganic powders such as ceramic powders will be pulverized and fragmented at ultra-high temperatures. Although a smooth and dense ceramic structure can be formed to retard the spread of flames, it is easy to crack and has poor self-molding performance. In order to further improve the high temperature resistance of the material, on the basis of adding ceramic powders, fiber materials are gradually introduced, such as ceramic composite tape / ceramic composite silicone foam formed by directly coating foam on glass fiber cloth and glass fiber mica paper, and reinforced silicone by directly mixing fibers in silicone. In recent years, fireproof and refractory materials have gradually developed in the direction of having a higher degree of compositeness in the hope of having better thermal runaway suppression performance.

[0003] Patent A method for preparing a fire-extinguishing ceramic silicone foam for pack battery pack (CN118359840A) discloses a method for preparing a fire-extinguishing ceramic silicone foam for pack battery pack. Silicone rubber is added to the ceramic silicone foam prepared to prepare a polymer composite material with tear-resistant and stretch-resistant effect, so that the polymer composite material has excellent tear-resistant performance in the preparation of ceramic silicone foam. With the addition of an anti-aging agent, the aging rate of the ceramic silicone foam during use is reduced, thereby increasing the durability and service life of the prepared ceramic silicone foam. At the same time, a flame retardant fire extinguishing agent is added to the raw material, and the flame retardant fire extinguishing agent is composed of 15 parts of antimony trioxide and 18 parts of zinc borate, so that the ceramic silicone foam will not easily burn during use, and it plays a role in flame retardant and fire extinguishing, and increases the safety of the ceramic silicone foam during use. Through the synergistic effect of multiple components, the silicone foam has a certain fire resistance, but after thermal runaway occurs, the ceramic silicone will quickly agglomerate and become brittle, or even powderized, and lose the effect of inhibiting the spread of thermal runaway.

[0004] Patent A glass fiber ceramic silicone sheet and its preparation process (CN118599320A) discloses a glass fiber ceramic silicone sheet and its preparation process. The glass fiber ceramic silicone sheet includes the following components by weight: 80-150 parts of silicone rubber matrix, 1-2 parts of cross-linking agent, 20-50 parts of fumed silica, 10-25 parts of modified filler, 5-10 parts of hydroxy silicone oil and 1-5 parts of vulcanizing agent. The modified filler adopts 5-ethylene-2-hydroxybenzoic acid modified glass fiber, so that it has good bonding force with the silicone body. When glass fiber is used as a reinforcing material for reinforced plastics, its biggest feature is its high tensile strength. Because its softening point is 500-750℃, it cannot effectively play a reinforcing role when thermal runaway occurs (temperature 1000C-1500C).

[0005] Patent A super-hard ceramic silica gel and its preparation method (CN117004226A) discloses a super-hard ceramic silica gel and its preparation method. The raw materials include 80-100 parts of silicone rubber, 5-15 parts of aluminum oxide, 10-15 parts of zirconium oxide, 2-10 parts of quartz powder, 15-20 parts of fiber small materials, 1-3 parts of hydroxy silicone oil, 0.5-2 parts of plasticizer, 0.5-1.5 parts of vulcanizing agent, wherein the fiber small materials are basalt fibers and treatment liquid (bismaleimide resin, palmitic acid and ether) mixed, stirred evenly and left to stand at room temperature for 2-3 hours to obtain fiber agglomerates and then dispersed, each fiber small material is composed of 3-6 irregularly bonded basalt short-cut fibers. It can effectively improve the ceramic degree of the material at high temperature, and also increase the hardness of the silica gel at room temperature, so that its rebound performance decreases.

[0006] Therefore, it is necessary to improve the existing technology to provide a more reliable solution. Summary of the invention

[0007] The technical problem to be solved by the present invention is to provide a fiber-reinforced fireproof silicone composite foam and a preparation method thereof in view of the deficiencies in the above-mentioned prior art.

[0008] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows: In the first aspect of the present invention, a fiber-reinforced fireproof silicone composite foam is provided, which is obtained by mixing component A and component B in a mass ratio of 0.5-2:0.5-2, coating, foaming and ripening, wherein the raw materials of component A include: vinyl silicone oil, platinum catalyst, powder filler, hydroxy silicone oil, and the mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil is 100: 0.025-0.1: 7.5-30: 2.5-10;

[0009] The raw materials of component B include: vinyl silicone oil, hydrogen-containing silicone oil, inhibitor, ceramic powder, fiber-reinforced base adhesive, and the mass ratio of vinyl silicone oil: hydrogen-containing silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive is 100: 4-16: 0.0015-0.006: 2.5-10: 5-50.

[0010] Preferably, the fiber-reinforced adhesive base is prepared by the following method:

[0011] Adding chopped fibers and a modifier into vinyl silicone oil, mixing them evenly and kneading them with silicone rubber to obtain a fiber-reinforced base rubber;

[0012] The mass ratio of chopped fiber to silicone rubber is 0.5-2:2.5-10, the mass of the modifier is 0.1-15% of the mass of the chopped fiber, and the mass of the vinyl silicone oil is 2-10 times of the mass of the chopped fiber.

[0013] Preferably, the chopped fibers are one or more of chopped high-silica glass fibers, chopped carbon fibers, chopped graphite fibers, chopped basalt fibers, and chopped aramid fibers.

[0014] Preferably, the modifier is one or more of γ-aminopropyltriethoxysilane, γ-glycidyloxypropyltrimethoxysilane, sodium dodecylbenzenesulfonate, γ-(methacryloyloxy)propyltrimethoxysilane, and maleic anhydride.

[0015] Preferably, the fiber-reinforced adhesive base is prepared by the following method:

[0016] Adding short-cut fibers and a modifier into vinyl silicone oil, stirring at 25 to 100 r / min for 1 to 4 hours, and then sand-milling in a sand mill at 100 to 400 r / min for 12 to 48 hours to obtain fiber pulp;

[0017] Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 to 60 rpm / min, and a stirring time of 0.2 to 3 hours; then, adjust the stirring speed to 30 to 200 rpm / min, heat to 100 to 170°C, stir for 1 to 24 hours, and take out to obtain a fiber-reinforced base rubber.

[0018] Preferably, in the component A, the mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil is 100:0.05:15:5.

[0019] Preferably, in the component B, the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive is 100:8:0.003:5:5-50.

[0020] Preferably, the mass ratio of component A to component B is 1:1.

[0021] A second aspect of the present invention provides a method for preparing the fiber-reinforced fire-resistant silica gel composite foam as described above, comprising the following steps:

[0022] S1. Mix component A and component B, stir, and obtain slurry;

[0023] S2. The slurry is coated on a release film, and after coating, vulcanization and foaming are performed at 80-85° C., and then aging is performed at 155-170° C. to obtain a fiber-reinforced fireproof silicone composite foam.

[0024] Preferably, the method for preparing the fiber-reinforced fireproof silica gel composite foam comprises the following steps:

[0025] S1. Mix component A and component B, and stir at a speed of 20-80 r / min for 2-3 min to obtain a slurry;

[0026] S2. Coat the slurry on the release film, and after coating, pass it through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 80°C; then pass it through 8 high-temperature vulcanization ovens for aging to obtain fiber-reinforced fire-proof silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155°C, 160°C, 170°C, 170°C, 170°C, 170°C, 170°C, 165°C; the length of each vulcanization oven and the high-temperature vulcanization oven is 2m, and the line speed of the whole machine during baking is 2.5m / min.

[0027] The beneficial effects of the present invention are:

[0028] The present invention provides a fiber-reinforced refractory silica gel foam and a preparation method thereof. Short-cut fibers are pretreated to prepare modified fiber pulp, which is then mixed with silica gel and foamed and vulcanized to prepare refractory silica gel foam. The synergistic effect of the modified fiber pulp and the ceramic powder in the silica gel foam is used to enhance the refractory performance of the foam, while retaining the resilience performance of the silica gel foam at room temperature.

[0029] In the present invention, by adding fiber materials into the silica gel foam, the foam not only has mechanical properties at room temperature, but also has fire-resistant and fire-insulating properties at high temperature;

[0030] In the present invention, by adding the fibers in the form of pulp, the dispersion of the fibers in the matrix is ​​improved, the fire resistance is better, and the addition amount is lower than that of short-cut fibers. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 This is a scanning electron microscope image of the fiber pulp prepared in Example 1;

[0032] Figure 2 Schematic diagram of the flame impact test. DETAILED DESCRIPTION

[0033] The present invention is further described in detail below in conjunction with embodiments so that those skilled in the art can implement the invention with reference to the description.

[0034] It should be understood that terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0035] The test methods used in the following examples are conventional methods unless otherwise specified. The materials and reagents used in the following examples are all commercially available unless otherwise specified. In the following examples, if no specific conditions are specified, the experiments were carried out under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used, if the manufacturer is not specified, are all conventional products that can be purchased commercially.

[0036] The present invention provides a fiber-reinforced fireproof silicone composite foam, which is obtained by mixing component A and component B in a mass ratio of 0.5-2:0.5-2, coating, foaming and ripening, wherein the raw materials of component A include: vinyl silicone oil, platinum catalyst, powder filler and hydroxy silicone oil, and the mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil is 100: 0.025-0.1: 7.5-30: 2.5-10;

[0037] The raw materials of component B include: vinyl silicone oil, hydrogen-containing silicone oil, inhibitor, ceramic powder, fiber-reinforced base adhesive, and the mass ratio of vinyl silicone oil: hydrogen-containing silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive is 100: 4-16: 0.0015-0.006: 2.5-10: 5-50.

[0038] In a preferred embodiment, the fiber-reinforced adhesive base is prepared by the following method:

[0039] Adding chopped fibers and a modifier into vinyl silicone oil, mixing them evenly and kneading them with silicone rubber to obtain a fiber-reinforced base rubber;

[0040] The mass ratio of chopped fiber to silicone rubber is 0.5-2:2.5-10, the mass of the modifier is 0.1-15% of the mass of the chopped fiber, and the mass of the vinyl silicone oil is 2-10 times of the mass of the chopped fiber.

[0041] The chopped fibers should have high temperature resistance and fire resistance. In a preferred embodiment, the chopped fibers are one or more of chopped high-silica glass fibers, chopped carbon fibers, chopped graphite fibers, chopped basalt fibers, and chopped aramid fibers.

[0042] In a preferred embodiment, the modifier is one or more of γ-aminopropyltriethoxysilane, γ-glycidyloxypropyltrimethoxysilane, sodium dodecylbenzenesulfonate, γ-(methacryloyloxy)propyltrimethoxysilane, and maleic anhydride.

[0043] In a preferred embodiment, the powder filler is specifically fumed silica.

[0044] In a preferred embodiment, the inhibitor is specifically HRO3.

[0045] In a preferred embodiment, the ceramic powder is specifically a mixture of aluminum oxide:silicon oxide in a mass ratio of 1:4.

[0046] In a preferred embodiment, the fiber-reinforced adhesive base is prepared by the following method:

[0047] Adding short-cut fibers and a modifier into vinyl silicone oil, stirring at 25 to 100 r / min for 1 to 4 hours, and then sand-milling in a sand mill at 100 to 400 r / min for 12 to 48 hours to obtain fiber pulp;

[0048] Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 to 60 rpm / min, and a stirring time of 0.2 to 3 hours; then, adjust the stirring speed to 30 to 200 rpm / min, heat to 100 to 170°C, stir for 1 to 24 hours, and take out to obtain a fiber-reinforced base rubber.

[0049] In a preferred embodiment, in component A, the mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil is 100:0.05:15:5.

[0050] In a preferred embodiment, in component B, the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive is 100:8:0.003:5:5-50.

[0051] In a preferred embodiment, the mass ratio of component A to component B is 1:1.

[0052] The present invention also provides a method for preparing the above fiber-reinforced fireproof silica gel composite foam, comprising the following steps:

[0053] S1. Mix component A and component B, stir, and obtain slurry;

[0054] S2. The slurry is coated on a release film, and after coating, vulcanization and foaming are performed at 80-85° C., and then aging is performed at 155-170° C. to obtain a fiber-reinforced fireproof silicone composite foam.

[0055] In a preferred embodiment, the method for preparing the fiber-reinforced fire-resistant silica gel composite foam comprises the following steps:

[0056] S1. Mix component A and component B, and stir at a speed of 20-80 r / min for 2-3 min to obtain a slurry;

[0057] S2. Coat the slurry on the release film, and after coating, pass it through 10-section vulcanization ovens for vulcanization and foaming. The temperatures of the 10 vulcanization ovens are set as 80°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 80°C in sequence; then pass it through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, so as to obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as 155°C, 160°C, 170°C, 170°C, 170°C, 170°C, 170°C, 165°C in sequence; the length of each vulcanization oven and the high-temperature vulcanization oven is 2m, and the line speed of the whole machine during baking is 2.5m / min.

[0058] The present invention makes the chopped fibers into pulp and premixes them with silicone rubber base, so that the chopped fibers have better dispersibility in silicone foam and less addition amount than the chopped fibers. The present invention uses the synergistic effect of the chopped fibers and the ceramic powder in the refractory silicone foam, so that the material has better fire resistance.

[0059] The above is the overall concept of the present invention, and detailed embodiments and comparative examples are provided below on the basis of the overall concept of the present invention to further illustrate the present invention.

[0060] The sources of some of the raw materials involved in the following examples and comparative examples are as follows:

[0061] Vinyl silicone oil (RH-Vi302) and hydrogenated silicone oil (RH-H45) were purchased from Ningbo Runhe High-tech Materials Technology Co., Ltd.; hydroxy silicone oil (viscosity 18000-22000 cSt) was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; silicone rubber (107 glue) was purchased from Foshan Huagu Silicone Co., Ltd.; platinum catalyst (DC-4000) was purchased from Guangzhou Weisheng Trading Co., Ltd.; inhibitor (HRO3) was purchased from Shenzhen Kejunchi Technology Co., Ltd.; ceramic powder (a mixture of alumina:silicon oxide in a mass ratio of 1:4) with a particle size of D50 = 30-50 um, homemade; powder filler (fumed silica A200) was purchased from Jinan Zhongbei Fine Chemical Co., Ltd.

[0063] Example 1

[0064] A fiber-reinforced fireproof silica gel composite foam, the preparation method of which comprises the following steps:

[0065] Step 1: Preparation of fiber reinforced adhesive base:

[0066] The chopped fibers and the modifier were added to the vinyl silicone oil, stirred at 50 r / min for 2 h, and then sand-milled in a sand mill at 200 r / min for 24 h to obtain fiber pulp; Figure 1 , is a scanning electron microscope image of the fiber pulp prepared in this embodiment, it can be seen that the fiber pulp is a slender fiber material with a diameter of 10 to 20 μm, which is dispersed in the matrix and provides a good reinforcement and toughening effect for the material;

[0067] Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 rpm / min, and a stirring time of 3 hours; then, adjust the stirring speed to 200 rpm / min, heat to 150°C, stir for 3 hours, and take out to obtain a fiber-reinforced base rubber.

[0068] The chopped fibers are chopped carbon fibers (with a length of 30 to 50 mm), the modifier is γ-aminopropyltriethoxysilane, and the mass of the modifier is 1% of the mass of the chopped fibers;

[0069] Among them, the mass ratio of chopped fiber: silicone rubber is 1:5, and the mass of vinyl silicone oil is 3 times the mass of chopped fiber.

[0070] Step 2: Prepare refractory silicone foam:

[0071] Ingredients:

[0072] Group A is mixed evenly according to the following raw material ratio: mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil = 100: 0.05: 15: 5;

[0073] The raw materials in group B are mixed evenly according to the following ratio: the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive = 100:8:0.003:5:20.

[0074] S1. Mix component A and component B in a mass ratio of 1:1 and add them into a planetary homogenizer. Stir for 3 minutes at a speed of 40 r / min to obtain a slurry. The uniformly mixed slurry should have no color difference.

[0075] S2. Coat the slurry on the release film and apply it through a calendering roller with a gap set at 0.500mm (i.e., the coating thickness is 0.5mm); after coating, pass through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 80℃; then pass through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, and obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155℃, 160℃, 170℃, 170℃, 170℃, 170℃, 170℃, 165℃; the length of each vulcanization oven and the high-temperature vulcanization oven is 2 meters, and the line speed of the whole machine during baking is 2.5m / min.

[0076] The density of the fireproof silicone composite foam prepared in this example is 500±50kg / m3; its properties are shown in Table 1.

[0077] Example 2

[0078] A fiber-reinforced fireproof silica gel composite foam, the preparation method of which comprises the following steps:

[0079] Step 1: Preparation of fiber reinforced adhesive base:

[0080] The chopped fibers and the modifier were added into the vinyl silicone oil, stirred at 50 r / min for 2 h, and then sand-milled in a sand mill at 500 r / min for 12 h to obtain fiber pulp;

[0081] Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 rpm / min, and a stirring time of 3 hours; then, adjust the stirring speed to 50 rpm / min, heat to 140°C, stir for 12 hours, and take out to obtain a fiber-reinforced base rubber.

[0082] The short-cut fibers are short-cut aramid fibers (length is 20 mm to 25 mm), the modifier is sodium dodecylbenzene sulfonate, and the mass of the modifier is 15% of the mass of the short-cut fibers;

[0083] Among them, the mass ratio of chopped fiber: silicone rubber is 1:3, and the mass of vinyl silicone oil is twice the mass of chopped fiber.

[0084] Step 2: Prepare refractory silicone foam:

[0085] Ingredients:

[0086] Group A is mixed evenly according to the following raw material ratio: mass ratio of vinyl silicone oil: platinum catalyst: fumed silica: hydroxy silicone oil = 100: 0.05: 15: 5;

[0087] The raw materials in group B are mixed evenly according to the following ratio: the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive = 100:8:0.003:5:50.

[0088] S1. Mix component A and component B in a mass ratio of 1:1 and add them into a planetary homogenizer. Stir for 3 minutes at a speed of 40 r / min to obtain a slurry. The uniformly mixed slurry should have no color difference.

[0089] S2. Coat the slurry on the release film and apply it through a calendering roller with a gap set at 0.6500mm; after coating, pass through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 80℃; then pass through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, and obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155℃, 160℃, 170℃, 170℃, 170℃, 170℃, 170℃, 165℃; the length of each vulcanization oven and the high-temperature vulcanization oven is 2 meters, and the line speed of the whole machine during baking is 2.5m / min.

[0090] The density of the fireproof silicone composite foam prepared in this example is 800±50kg / m 3 ; Its performance is shown in Table 1.

[0091] Example 3

[0092] A fiber-reinforced fireproof silica gel composite foam, the preparation method of which comprises the following steps:

[0093] Step 1: Preparation of fiber reinforced adhesive base:

[0094] The chopped fibers and the modifier were added into the vinyl silicone oil, stirred at 50 r / min for 2 h, and then sand-milled in a sand mill at 500 r / min for 12 h to obtain fiber pulp;

[0095] Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 rpm / min, and a stirring time of 3 hours; then, adjust the stirring speed to 150 rpm / min, heat to 170°C, stir for 24 hours, and take out to obtain a fiber-reinforced base rubber.

[0096] The chopped fibers are a mixture of basalt fibers (20-25 mm in length) and PAN fibers (40-50 mm in length) in a mass ratio of 1:1, and the modifier is γ-glycidyloxypropyltrimethoxysilane, the mass of which is 3% of the mass of the chopped fibers.

[0097] Among them, the mass ratio of chopped fiber: silicone rubber is 1:10, and the mass of vinyl silicone oil is 10 times the mass of chopped fiber.

[0098] Step 2: Prepare refractory silicone foam:

[0099] Ingredients:

[0100] Group A is mixed evenly according to the following raw material ratio: mass ratio of vinyl silicone oil: platinum catalyst: fumed silica: hydroxy silicone oil = 100: 0.05: 15: 5;

[0101] The raw materials in group B are mixed evenly according to the following ratio: the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive = 100:8:0.003:5:30.

[0102] S1. Mix component A and component B in a mass ratio of 1:1 and add them into a planetary homogenizer. Stir for 3 minutes at a speed of 40 r / min to obtain a slurry. The uniformly mixed slurry should have no color difference.

[0103] S2. Coat the slurry on the release film and apply it through a calendering roller with a gap set at 0.5500mm; after coating, pass through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 80℃; then pass through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, and obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155℃, 160℃, 170℃, 170℃, 170℃, 170℃, 170℃, 165℃; the length of each vulcanization oven and the high-temperature vulcanization oven is 2 meters, and the line speed of the whole machine during baking is 2.5m / min.

[0104] The density of the fireproof silicone composite foam prepared in this example is 700±50kg / m 3 ; Its performance is shown in Table 1.

[0105] Example 4

[0106] A fiber-reinforced fireproof silica gel composite foam, the preparation method of which comprises the following steps:

[0107] Step 1: Preparation of fiber reinforced adhesive base:

[0108] The short-cut fibers and the modifier are added into the vinyl silicone oil, stirred at 50 r / min for 2 h, and then sand-milled in a sand mill at 500 r / min for 6 h to obtain fiber pulp;

[0109] Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 rpm / min, and a stirring time of 3 hours; then, adjust the stirring speed to 150 rpm / min, heat to 100°C, stir for 3 hours, and take out to obtain a fiber-reinforced base rubber.

[0110] The chopped fibers are a mixture of chopped aramid (30-50 mm in length): chopped glass fibers (30-50 mm in length): chopped carbon fibers (30-50 mm in length) in a mass ratio of 2:1:1, and the modifier is a mixture of γ-(methacryloyloxy)propyltrimethoxysilane: maleic anhydride in a mass ratio of 2:1, and the mass of the modifier is 0.5% of the mass of the chopped fibers;

[0111] Among them, the mass ratio of chopped fiber: silicone rubber is 1:4, and the mass of vinyl silicone oil is 6 times the mass of chopped fiber.

[0112] Step 2: Prepare refractory silicone foam:

[0113] Ingredients:

[0114] Group A is mixed evenly according to the following raw material ratio: mass ratio of vinyl silicone oil: platinum catalyst: fumed silica: hydroxy silicone oil = 100: 0.05: 15: 5;

[0115] The raw materials in group B are mixed evenly according to the following ratio: the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive = 100:8:0.003:5:30.

[0116] S1. Mix component A and component B in a mass ratio of 1:1 and add them into a planetary homogenizer. Stir for 3 minutes at a speed of 40 r / min to obtain a slurry. The uniformly mixed slurry should have no color difference.

[0117] S2. Coat the slurry on the release film and apply it through a calendering roller with a gap set at 0.700mm; after coating, pass through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 80℃; then pass through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, and obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155℃, 160℃, 170℃, 170℃, 170℃, 170℃, 170℃, 165℃; the length of each vulcanization oven and the high-temperature vulcanization oven is 2 meters, and the line speed of the whole machine during baking is 2.5m / min.

[0118] The density of the fireproof silicone composite foam prepared in this example is 900±50kg / m3 ; Its performance is shown in Table 1.

[0119] Comparative Example 1

[0120] A fiber-reinforced fireproof silica gel composite foam, the preparation method of which comprises the following steps:

[0121] Ingredients:

[0122] Group A is mixed evenly according to the following raw material ratio: mass ratio of vinyl silicone oil: platinum catalyst: fumed silica: hydroxy silicone oil = 100: 0.05: 15: 5;

[0123] The raw materials of group B are mixed evenly according to the following ratio: the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: silicone rubber = 100:8:0.003:5:30.

[0124] S1. Mix component A and component B in a mass ratio of 1:1 and add them into a planetary homogenizer. Stir for 3 minutes at a speed of 40 r / min to obtain a slurry. The uniformly mixed slurry should have no color difference.

[0125] S2. Coat the slurry on the release film and apply it through a calendering roller with a gap set at 0.6000mm; after coating, pass through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 80℃; then pass through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, and obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155℃, 160℃, 170℃, 170℃, 170℃, 170℃, 170℃, 165℃; the length of each vulcanization oven and the high-temperature vulcanization oven is 2 meters, and the line speed of the whole machine during baking is 2.5m / min.

[0126] The density of the fireproof silicone composite foam prepared in this example is 700±50kg / m 3 ; Its performance is shown in Table 1.

[0127] Comparative Example 2

[0128] A fiber-reinforced fireproof silica gel composite foam, the preparation method of which comprises the following steps:

[0129] Step 1: Preparation of fiber reinforced adhesive base:

[0130] The chopped fibers and silicone rubber were added to a kneader for mixing at a vacuum degree of -0.1 MPa, a rotation speed of 10 rpm / min, and a stirring time of 3 hours. Afterwards, the stirring speed was adjusted to 150 rpm / min, and the mixture was heated to 100°C and stirred for 3 hours. The mixture was taken out to obtain a fiber-reinforced base rubber.

[0131] Among them, the chopped fibers are chopped glass fibers (length 30 to 50 mm);

[0132] The mass ratio of chopped fiber to silicone rubber is 1:4.

[0133] Step 2: Prepare refractory silicone foam:

[0134] Ingredients:

[0135] Group A is mixed evenly according to the following raw material ratio: mass ratio of vinyl silicone oil: platinum catalyst: fumed silica: hydroxy silicone oil = 100: 0.05: 15: 5;

[0136] The raw materials in group B are mixed evenly according to the following ratio: the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive = 100:8:0.003:5:60.

[0137] S1. Mix component A and component B in a mass ratio of 1:1 and add them into a planetary homogenizer. Stir for 3 minutes at a speed of 40 r / min to obtain a slurry. The uniformly mixed slurry should have no color difference.

[0138] S2. Coat the slurry on the release film and apply it through a calendering roller with a gap set at 0.6500mm; after coating, pass through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 85℃, 80℃; then pass through 8 high-temperature vulcanization ovens for aging to ensure that the finished product has stable mechanical, flame retardant and other properties, and obtain fiber-reinforced fire-resistant silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155℃, 160℃, 170℃, 170℃, 170℃, 170℃, 170℃, 165℃; the length of each vulcanization oven and the high-temperature vulcanization oven is 2 meters, and the line speed of the whole machine during baking is 2.5m / min.

[0139] The density of the fireproof silicone composite foam prepared in this example is 700±50kg / m 3 ; Its performance is shown in Table 1.

[0140] Table 1 Comparison of the performance of silicone foam in the embodiment and the comparative example (tensile properties, flame retardant properties, fire resistance), the total thickness of the foam is 3 mm;

[0141]

[0142] Flame impact test method reference Figure 2 The flame impact test distance was d=100mm for 800℃ and d=50mm for 1300℃.

[0143] According to the test results in Table 1, it can be seen that adding reinforcing fibers to silicone foam can effectively improve the fire resistance of the foam during flame impact. After the fibers are processed into pulp, they are more evenly dispersed in the matrix and the reinforcing effect is more obvious. The effects of fibers of different materials are slightly different. The fiber pulp made of carbon fiber and basalt fiber has better effects.

[0144] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.

Claims

1. A fiber-reinforced fireproof silica gel composite foam, characterized in that: The invention is obtained by mixing component A and component B in a mass ratio of 0.5-2:0.5-2, coating, foaming and ripening. The raw materials of component A include: vinyl silicone oil, platinum catalyst, powder filler and hydroxy silicone oil. The mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil is 100: 0.025-0.1: 7.5-30: 2.5-10. The raw materials of component B include: vinyl silicone oil, hydrogen-containing silicone oil, inhibitor, ceramic powder, fiber-reinforced base adhesive, and the mass ratio of vinyl silicone oil: hydrogen-containing silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive is 100: 4-16: 0.0015-0.006: 2.5-10: 5-50.

2. The fiber-reinforced fireproof silica composite foam according to claim 1, characterized in that: The fiber-reinforced adhesive base is prepared by the following method: Adding chopped fibers and a modifier into vinyl silicone oil, mixing them evenly and kneading them with silicone rubber to obtain a fiber-reinforced base rubber; The mass ratio of chopped fiber to silicone rubber is 0.5-2:2.5-10, the mass of the modifier is 0.1-15% of the mass of the chopped fiber, and the mass of the vinyl silicone oil is 2-10 times of the mass of the chopped fiber.

3. The fiber-reinforced fireproof silica composite foam according to claim 2, characterized in that: The chopped fibers are one or more of chopped high-silica glass fibers, chopped carbon fibers, chopped graphite fibers, chopped basalt fibers, and chopped aramid fibers.

4. The fiber-reinforced fireproof silica composite foam according to claim 2, characterized in that: The modifier is one or more of γ-aminopropyltriethoxysilane, γ-glycidyloxypropyltrimethoxysilane, sodium dodecylbenzenesulfonate, γ-(methacryloyloxy)propyltrimethoxysilane and maleic anhydride.

5. The fiber-reinforced fireproof silica composite foam according to claim 2, characterized in that: The fiber-reinforced adhesive base is prepared by the following method: Adding short-cut fibers and a modifier into vinyl silicone oil, stirring at 25 to 100 r / min for 1 to 4 hours, and then sand-milling in a sand mill at 100 to 400 r / min for 12 to 48 hours to obtain fiber pulp; Add the fiber pulp and silicone rubber into a kneader for mixing, with a vacuum degree of -0.1 MPa, a rotation speed of 10 to 60 rpm / min, and a stirring time of 0.2 to 3 hours; then, adjust the stirring speed to 30 to 200 rpm / min, heat to 100 to 170°C, stir for 1 to 24 hours, and take out to obtain a fiber-reinforced base rubber.

6. The fiber-reinforced fireproof silica composite foam according to claim 1, characterized in that: In the component A, the mass ratio of vinyl silicone oil: platinum catalyst: powder filler: hydroxy silicone oil is 100:0.05:15:

5.

7. The fiber-reinforced fireproof silica composite foam according to claim 1, characterized in that: In the component B, the mass ratio of vinyl silicone oil: hydrogenated silicone oil: inhibitor: ceramic powder: fiber-reinforced base adhesive is 100:8:0.003:5:5-50.

8. The fiber-reinforced fireproof silica composite foam according to claim 1, characterized in that: The mass ratio of component A to component B is 1:

1.

9. A method for preparing the fiber-reinforced fireproof silica gel composite foam as claimed in any one of claims 1 to 8, characterized in that: The following steps are involved: S1. Mix component A and component B, stir, and obtain slurry; S2. The slurry is coated on a release film, and after coating, vulcanization and foaming are performed at 80-85° C., and then aging is performed at 155-170° C. to obtain a fiber-reinforced fireproof silicone composite foam.

10. The method for preparing the fiber-reinforced fireproof silica gel composite foam according to claim 9, characterized in that: The following steps are involved: S1. Mix component A and component B, and stir at a speed of 20-80 r / min for 2-3 min to obtain a slurry; S2. Coat the slurry on the release film, and after coating, pass it through 10-section vulcanization ovens for vulcanization and foaming, and the temperatures of the 10 vulcanization ovens are set as follows: 80°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 85°C, 80°C; then pass it through 8 high-temperature vulcanization ovens for aging to obtain fiber-reinforced fire-proof silicone composite foam, wherein the temperatures of the high-temperature vulcanization ovens are set as follows: 155°C, 160°C, 170°C, 170°C, 170°C, 170°C, 170°C, 165°C; the length of each vulcanization oven and the high-temperature vulcanization oven is 2m, and the line speed of the whole machine during baking is 2.5m / min.

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