Application of Terminal Alkenyl Heptaphenyl POSS in the Preparation of Ceramed Organosilicon Thermal Insulation Materials

Abstract

The present invention relates to the field of composite materials. The present invention discloses the application of terminal alkenyl heptaphenyl POSS in the preparation of ceramizable silicone heat insulation materials. First of all, the present invention uses terminal alkenyl heptaphenyl POSS as a raw material to prepare an injectable ceramizable silicone heat insulation material, which can effectively reduce the viscosity of the raw materials of the ceramizable silicone heat insulation material, so that it can be prepared by injection molding. Secondly, the raw materials of the ceramizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS of the present invention contain phenyl silicone resin with low molecular weight side chain hanging alkenyl, cobalt-zinc ferrite complex and terminal alkenyl heptaphenyl POSS, which can have both high heat insulation and high heat resistance and can be applicable to the injection molding process. The material obtained by the injection molding process can be used for the coating of soft copper busbar insulated wires, which can improve the space utilization rate of the battery pack and the energy density of the power battery.

Description

Technical Field

[0001] The present invention relates to the field of composite materials, and particularly relates to an end-alkenyl heptaphenyl POSS and its application in the preparation of ceramizable silicone thermal insulation materials. Background Art

[0002] The sales volume of new energy vehicles is increasing day by day, but the problems of overheating and fire still remain a lingering shadow for manufacturers and consumers. Insulating and heat-insulating the copper busbar connection wires responsible for transmitting electric energy is one of the effective ways to avoid the fire of electric vehicles. The existing treatment solutions for copper busbar connection wires mainly focus on heat shrinkable tubes and insulating resin spraying. The disadvantages of heat shrinkable tubes and insulating resins are their limited temperature resistance. When the battery is thermally out of control and exposed to high temperature or flame, they are prone to decompose and form ashes, thus losing their insulating and fireproof capabilities and failing to meet the fireproof requirements of the vehicle manufacturers. Even if a layer of high-temperature resistant fiberglass tape is bundled outside the insulating resin or heat shrinkable tube, the problem that the protective layer is prone to peeling off under the impact of high-temperature flame and the insulation fails still cannot be solved.

[0003] Ceramizable silicone rubber is currently an ideal high-temperature resistant insulating material. Ceramizable silicone rubber is inherently heat-resistant and insulating, and when burning, the silicon-oxygen structural units will turn into continuous, antioxidant, and insulating network-like silica ashes covering the surface. It can not only prevent further ablation, but also these silica ashes can undergo eutectic reaction with refractory fillers to generate a dense and relatively strong high-temperature resistant ceramic layer, thereby achieving the purpose of flame retardancy, fire resistance, and insulation.

[0004] Currently, the commonly used molding process for ceramized silicone rubber is the compression molding process. For example, Chinese invention patent CN202111273551.1 discloses a ceramized silicone rubber for thermal insulation of power batteries and its preparation method. The ceramized silicone rubber comprises the following raw materials in parts by weight: 100 parts of silica gel, 5 - 20 parts of zinc borate, 6 - 15 parts of alumina, 5 - 10 parts of mica powder, 3 - 5 parts of kaolin, 10 - 25 parts of glass powder, 0.1 - 0.4 parts of silane coupling agent, 5 - 20 parts of silicone oil, 20 - 30 parts of white carbon black, 4 - 10 parts of magnesium oxide, and 10 - 20 parts of ceramic fiber. The preparation method is to weigh the raw materials and mix them into a powder, followed by kneading and stirring, cooling and aging, sulfur addition and open milling, tablet pressing, and finally heating and vulcanization molding to obtain the ceramized silicone rubber. Chinese invention patent CN202110350619.5 discloses a thermally conductive ceramized silicone rubber material and its preparation method. This material is obtained by adding a composite ceramization filler, a flame retardant, and a vulcanizing agent to a silicone rubber matrix and performing high-temperature compression vulcanization. The disadvantage of the compression molding process is low efficiency, a large amount of rubber compound loss during production, and the need to remove flash after demolding, resulting in limited production capacity. Moreover, the compression molding process is not suitable for soft copper bars that play a positive role in improving the energy density of power battery packs. However, if an injection molding process is used to coat the soft copper bar with an organosilicon thermal insulation material on the outside, the above technical problems can be solved. However, existing resins for injection molding require a lower viscosity, while the viscosity of traditional phenyl silicone resins for preparing ceramized silicone rubber is generally high. Therefore, direct injection molding will have problems with difficult processing.

[0005] In summary, it is of positive significance to develop a ceramized organosilicon thermal insulation material with excellent heat insulation, heat resistance, and applicability to injection molding. Summary of the Invention

[0006] First, to solve the technical problem that traditional phenyl silicone resins cannot be used to prepare ceramized organosilicon thermal insulation materials through the injection molding process, the present invention provides an application of terminal alkenyl heptaphenyl POSS in the preparation of ceramized organosilicon thermal insulation materials. Terminal alkenyl heptaphenyl POSS can effectively reduce the viscosity of the raw materials of ceramized organosilicon thermal insulation materials, enabling them to be prepared by injection molding. Second, to solve the technical problem that existing ceramized organosilicon thermal insulation materials are difficult to have both high heat insulation, high heat resistance and insulation, and applicability to injection molding, the present invention provides a ceramized organosilicon thermal insulation material containing terminal alkenyl heptaphenyl POSS. The raw materials of this material contain a phenyl silicone resin with low molecular weight side chain pendant alkenyl groups, a cobalt zinc ferrite complex, and terminal alkenyl heptaphenyl POSS, and a ceramized organosilicon thermal insulation material with both high heat insulation and high heat resistance can be prepared by the injection molding process.

[0007] The specific technical solution of the present invention is as follows:

[0008] In a first aspect, the present invention provides an application of an alkenyl heptaphenyl POSS in the preparation of an injectable ceramifiable silicone heat insulation material and an application in improving the injection molding process adaptability of a ceramifiable silicone heat insulation material. The structural formula of the alkenyl heptaphenyl POSS is as follows:

[0009]

[0010] Wherein, n = 0 - 9, more preferably 3 - 6.

[0011] The present invention discovers that by introducing the alkenyl heptaphenyl POSS into the ceramifiable silicone heat insulation material through hydrosilylation, after grafting the bulky phenyl POSS onto the main chain of the polymer, the intermolecular force can be reduced, the viscosity of the resin reaction system can be significantly reduced, changing the high-viscosity situation of traditional phenyl silicone resins, which is beneficial to the preparation of ceramifiable silicone heat insulation materials by injection molding process.

[0012] In addition, by controlling the introduction amount and type of the alkenyl heptaphenyl POSS, the crosslinking density of the ceramifiable silicone heat insulation material can be adjusted, and the heat resistance of the material can be significantly improved by using the inorganic / organic hybrid enhanced heat insulation and heat resistance effect.

[0013] Furthermore, the present invention preferably has the carbon chain length containing an alkenyl group in the alkenyl heptaphenyl POSS being 5 - 8 (including the alkenyl group). The reason is that we find that due to the huge volume of phenyl POSS, if the carbon chain length is too short, the alkenyl group is easily shielded by phenyl POSS and cannot fully participate in the addition reaction due to steric hindrance effect and the increase in the molecular weight of the main chain during the reaction, resulting in low grafting efficiency. On the contrary, if the carbon chain length is too long, the inorganic-organic synergistic effect is reduced, which is also likely to lead to too high viscosity of the compound, thus reducing the viscosity reduction effect of the alkenyl heptaphenyl POSS. Therefore, appropriately increasing the carbon chain arm length can make the alkenyl group fully extend and avoid interference from phenyl POSS.

[0014] Preferably, the preparation route of the alkenyl heptaphenyl POSS is as follows:

[0015]

[0016] Preferably, the preparation method of the alkenyl heptaphenyl POSS includes: adding an organic solvent, sodium hydroxide and water into a reactor and stirring evenly, dropping phenyltriethoxysilane, heating to reflux after dropping, reacting; after cooling, vacuum removing the organic solvent, adding another organic solvent to dissolve, cooling to -5 to 0 °C, adding pyridine, dropping alkenyltrichlorosilane with a carbon chain length of 2 - 11 for reaction, and heating to continue the reaction to obtain the alkenyl heptaphenyl POSS.

[0017] The present invention uses phenylsiloxane to prepare phenyl T7 trisiloxane, and then uses the method of corner - missing closed - loop to prepare terminal - alkenyl heptaphenyl POSS. Among them, the role of pyridine is to absorb HCl that appears during the reaction, making the synthesis of terminal - alkenyl heptaphenyl POSS more complete.

[0018] In a second aspect, the present invention provides an injectable ceramizable silicone thermal insulation material based on terminal - alkenyl heptaphenyl POSS, which is obtained by uniformly mixing components including component A and component B and then heating and curing; wherein:

[0019] Component A includes the following raw materials: hydrogen - containing silicone oil, silica aerogel, cobalt - zinc - ferrite complex, hollow glass microspheres, reaction rate regulator.

[0020] In component A, hydrogen - containing silicone oil is one of the cross - linking agent components; the combination of silica aerogel, cobalt - zinc - ferrite complex and hollow glass microspheres can synergistically exert a heat - insulation effect; in addition, silica aerogel also has the function of reinforcing the resin. The reaction rate regulator is used to control the reaction time.

[0021] Component B includes the following raw materials: phenyl silicone resin with low - molecular - weight side - chain - hanging alkenyl groups, terminal - alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt - zinc - ferrite complex, dispersion promoter, catalyst.

[0022] In component B, phenyl silicone resin with low - molecular - weight side - chain - hanging alkenyl groups and terminal - alkenyl heptaphenyl POSS are used as main cross - linking agents; the combination of silica aerogel, spherical alumina, cobalt - zinc - ferrite complex can synergistically exert a heat - insulation effect; the catalyst is used to promote the occurrence of the reaction.

[0023] After uniformly mixing component A and component B and heating and curing by injection molding, the ceramizable silicone thermal insulation material based on terminal - alkenyl heptaphenyl POSS can be obtained, and its curing mechanism is as follows:

[0024]

[0025] During the above - mentioned curing reaction process, under the action of the catalyst, hydrogen - containing silicone oil, phenyl silicone resin with low - molecular - weight side - chain - hanging alkenyl groups and terminal - alkenyl heptaphenyl POSS undergo a hydrosilylation reaction. The formed silicone thermal insulation material has a three - dimensional cross - linked network structure microscopically. Among them, inorganic particles such as silica aerogel, cobalt - zinc - ferrite complex, hollow glass microspheres and spherical alumina, as well as cage - shaped POSS, are dispersedly "embedded" in the grid pores of the three - dimensional network structure, thus endowing the material with excellent heat - insulation performance. The reaction rate regulator is used to control the reaction time for the formation of the three - dimensional cross - linked network structure, avoiding too fast cross - linking reaction rate, uneven distribution of inorganic materials in the three - dimensional network structure, and affecting the heat - insulation effect of the material.

[0026] In the raw materials of the ceramized silicone heat-insulating material of the present invention, there are simultaneously phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups, cobalt zinc ferrite complex, and terminal alkenyl heptaphenyl POSS. Its technical effects are as follows: 1) Make full use of the inorganic / organic hybrid enhancement of heat insulation and heat resistance effects. The terminal alkenyl heptaphenyl POSS is introduced into the reaction system by hydrosilylation. By controlling the introduction amount and type, the crosslinking density is optimized to an appropriate level, and without significantly increasing the viscosity of the raw materials, the heat insulation and heat resistance of the silicone material are significantly improved. 2) Utilize the viscosity reduction effect of large groups on the side chains of polymers. The huge phenyl POSS is grafted onto the main chain of the polymer, reducing the intermolecular force, changing the high-viscosity situation of traditional phenyl silicone resin, reducing the viscosity of the resin reaction system, and facilitating the rapid injection molding of the silicone heat-insulating material. 3) Utilize the inorganic-inorganic synergistic ceramic-forming effect. Introduce a cobalt zinc ferrite complex with a spinel structure, which synergistically embeds with the silica aerogel into the three-dimensional crosslinked network structure of the material, forming a dense and continuous structure in a rivet networking manner, and it is easier to rapidly form ceramics during the combustion of the material when encountering fire. In addition, both the cobalt zinc ferrite complex and the silica aerogel have excellent heat resistance, and the heat resistance performance is better than that of a single system.

[0027] Preferably, the component A includes the following raw materials in mass percentages: hydrogen-containing silicone oil 20 - 50%, silica aerogel 5 - 25%, cobalt zinc ferrite complex 5 - 25%, hollow glass microspheres 5 - 20%, reaction rate regulator 0 - 1%.

[0028] Preferably, the component B includes the following raw materials in mass percentages: phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups 20 - 45%, terminal alkenyl heptaphenyl POSS 5 - 15%, silica aerogel 5 - 25%, spherical alumina 5 - 25%, cobalt zinc ferrite complex 15 - 25%, dispersion promoter 1 - 5%, catalyst 0.1 - 0.3%.

[0029] It should be noted that the present invention finds that the introduction amount of terminal alkenyl heptaphenyl POSS will have a significant impact on the performance of the material. If the content is too low, the modification effect is not good, while if the content is too high, the resin is prone to cracking after curing. Therefore, preferably, the present invention finds that controlling the content of terminal alkenyl heptaphenyl POSS at 5 - 15% can solve the above technical problems.

[0030] Preferably, the mass ratio of the component A to the component B is 1.5 - 2.5∶1.

[0031] Preferably, the structural formula of the phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups is as follows:

[0032]

[0033] Among them, X is 4 - 10.

[0034] The present invention finds that the molecular weight of the phenyl silicone resin with vinyl groups hanging on the side chain is also crucial for whether the final material is suitable for injection molding processing. If the molecular chain is too long and the molecular weight is too large, the intermolecular force is strong, the resin viscosity is high, which is not conducive to injection molding processing. Finally, it is found that within the range of X = 4 - 10, good injectability can be imparted to the material.

[0035] Preferably, the preparation method of the low - molecular - weight phenyl silicone resin with vinyl groups hanging on the side chain has the following synthetic route:

[0036]

[0037] Among them, X is 4 - 10.

[0038] Preferably, the preparation method of the low - molecular - weight phenyl silicone resin with vinyl groups hanging on the side chain includes: in an inert gas atmosphere with a water content of 0.05 - 0.1 wt%, methylphenyl dichlorosilane, methylvinyl dichlorosilane and diphenyldiethoxysilane are mixed evenly and dropped into a reaction system with an ice - salt bath, the temperature is controlled at - 25~ - 15 °C. After dropping, the reaction continues for 4 - 8 h, during which the generated HCl is separated. The inert gas protection is removed, and the temperature is raised to room temperature. After continuing the reaction for 4 - 8 h, trimethylchlorosilane is dropped for end - capping reaction. After dropping, the temperature is raised to 70 - 90 °C, and the reaction continues for 10 - 15 h. Then, low - boiling substances are removed by vacuum distillation, and then the temperature is raised to 140 - 160 °C for structural rearrangement for 20 - 30 h to obtain the low - molecular - weight phenyl silicone resin with vinyl groups hanging on the side chain.

[0039] In the above - mentioned preparation process of the present invention, chlorosilane is very active and decomposes when encountering water vapor in the air, generating silanol and hydrogen chloride gas. Under acidic conditions, silanol will further undergo a condensation reaction with alkoxysilane to produce small - molecule organosilicon polymers and release ethanol. In order to control the hydrolysis rate of chlorosilane, the present invention selects to carry out the reaction under the protection of a water - containing inert gas (preferably nitrogen). It should be noted that the water content of the inert gas is crucial. An appropriate water content can make chlorosilane hydrolyze slowly. If the water content is too low, hydrolysis cannot occur smoothly; on the contrary, if the water content is too high, the hydrolysis rate is likely to be too fast, resulting in gelation of the product. At the same time, the continuously flowing inert gas can carry out the generated hydrogen chloride gas, promoting the continuous and stable progress of the reaction. In the subsequent steps under room - temperature conditions and above, the inert gas protection needs to be removed in time, otherwise it will affect the progress of the subsequent reaction.

[0040] Preferably, the molar ratio of methylphenyldichlorosilane, methylvinyldichlorosilane, diphenyldiethoxysilane and trimethylchlorosilane is (0.7 - 0.9)∶(0.1 - 0.3)∶(0.8 - 1.2)∶(0.1 - 0.3).

[0041] Preferably, the cobalt-zinc ferrite complex is CoZnFe 4 O 8 .

[0042] Preferably, the preparation reaction formula of the cobalt-zinc ferrite complex is: 4Fe(NO 3 ) 3 + Co(NO 3 ) 2 + 7O 2 + Zn(NO 3 ) 2 + 6C 6 H 8 O 7 → CoZnFe 4 O 8 + 8N 2 + 36CO 2 + 24H 2 O.

[0043] More preferably, the preparation method of the cobalt-zinc ferrite complex specifically includes: fully dissolving iron nitrate, cobalt nitrate, zinc nitrate and citric acid in water, heating to 85 - 95 °C, reacting under the bubbling action of a continuous air stream and continuously replenishing water, and obtaining the cobalt-zinc ferrite complex after filtration and drying.

[0044] The present invention uses the sol-gel precipitation method to prepare the cobalt-zinc ferrite complex in one step. The process is simple, the product has good stability, and the prepared complex has a spinel structure.

[0045] Preferably, the reaction rate regulator is composed of butyl succinic anhydride and 3,5-propyl-1-butyne-3-ol with an excess of alcohol.

[0046] In the hydrosilylation reaction during the injection molding and curing stage of the present invention, platinum catalysts such as Karstedt are very active, and the reaction is intense and prone to gelation. To reduce the reaction rate, reagents that can slow down the reaction rate usually need to be added. However, after adding these reagents, while the reaction rate is reduced, it is not conducive to injection molding. Therefore, one of the key points for injectable molding is how to trigger the catalytic rapid curing reaction. After reaching the triggering temperature, the silicone resin rapidly forms, resulting in a ceramized silicone heat insulation material. The solution provided by the present invention is to use temperature-responsive butyl succinic anhydride (phase transition temperature of 46 °C) to react with 3,5-propyl-1-butyn-3-ol that can slow down the reaction (the ring-opening of butyl succinic anhydride forms an acid) to control the concentration of 3,5-propyl-1-butyn-3-ol in the reaction system. When the temperature is higher than 50 °C, butyl succinic anhydride changes from a solid state to a liquid state, increasing the reaction rate with 3,5-propyl-1-butyn-3-ol, rapidly consuming 3,5-propyl-1-butyn-3-ol, releasing the efficiency of the catalyst, and the organic acid generated by this reaction can further improve the efficiency of the catalyst, thereby achieving temperature-responsive triggering of catalytic rapid curing.

[0047] Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.1-2.0 wt%; the dispersion promoter is isopropoxy tris(p-aminophenoxy) titanate; the catalyst is a platinum catalyst.

[0048] In a third aspect, the present invention provides a method for preparing an injectable ceramized silicone heat insulation material of the above-mentioned terminal alkenyl heptaphenyl POSS, comprising the following steps:

[0049] S1: Preparation of component A: Mix the hydrogen-containing silicone oil, silica aerogel, cobalt-zinc ferrite complex, hollow glass microspheres, and reaction rate regulator evenly to obtain component A;

[0050] S2: Preparation of component B: Mix the phenyl silicone resin with low molecular weight side-chain pendant alkenyl groups, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt-zinc ferrite complex, dispersion promoter, and catalyst evenly to obtain component B;

[0051] S3: Mix component A and component B evenly and heat for curing.

[0052] Preferably, in S1, the hydrogen-containing silicone oil, silica aerogel, cobalt-zinc ferrite complex, hollow glass microspheres, and reaction rate regulator are mixed and stirred evenly for 1-3 h under the conditions of a temperature lower than 40 °C and a vacuum degree of -0.01 to -0.1 Mpa to obtain component A.

[0053] Preferably, in S2, a phenyl silicone resin with low-molecular-weight side-chain pendant alkenyl, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt-zinc ferrite composite, dispersion promoter, and catalyst are mixed and stirred evenly for 1-3 h under the conditions of a temperature below 60 °C and a vacuum degree of -0.01 to -0.1 Mpa to obtain Component B.

[0054] Preferably, in S3, Component A and Component B are mixed evenly and heated to 50-90 °C for curing, and the curing is completed within 3 min.

[0055] Compared with the prior art, the present invention has the following technical effects:

[0056] (1) The present invention discovers that by introducing terminal alkenyl heptaphenyl POSS into the ceramizable silicone thermal insulation material through hydrosilylation, after grafting the huge phenyl POSS onto the main chain of the polymer, the intermolecular force can be reduced, and the viscosity of the resin reaction system can be significantly reduced, which is beneficial to the preparation of ceramizable silicone thermal insulation materials by injection molding process.

[0057] (2) The present invention uses phenylsiloxane to prepare phenyl T7 trisiloxane, then uses the corner-cut closed-loop method to prepare terminal alkenyl heptaphenyl POSS, and then incorporates it into the reaction system through hydrosilylation. By controlling the introduction amount and type, the crosslinking density is adjusted, and the inorganic / organic hybrid enhanced heat insulation and heat resistance effects are fully utilized, so that the heat resistance of the thermal insulation material can be significantly improved.

[0058] (3) By limiting the carbon chain length of the terminal alkenyl in terminal alkenyl heptaphenyl POSS, the present invention can not only prevent the terminal alkenyl from being interfered by phenyl POSS in the addition reaction, but also avoid the too high viscosity of terminal alkenyl heptaphenyl POSS itself and its polymerized polymer.

[0059] (4) The present invention uses the sol-gel precipitation method to prepare cobalt-zinc ferrite composite in one step. The process is simple and the product has good stability. The prepared composite has a spinel structure, which can be synergistically embedded into the three-dimensional crosslinked network structure of the material with silica aerogel to form a dense and continuous structure in the way of riveting and networking, making use of the inorganic-inorganic synergistic porcelain-forming effect and being more likely to form porcelain quickly under high-temperature conditions. In addition, both cobalt-zinc ferrite composite and silica aerogel have excellent heat resistance, and their heat resistance performance is better than that of a single system.

[0060] (5) The injection liquid viscosity of the raw material of the ceramizable thermal insulation material of the present invention is low, which is suitable for the injection molding process. Therefore, the product has high precision and less flash, improving the production efficiency. In addition, this material can be used for the coating of soft copper busbar insulated wires, which can improve the space utilization rate of the battery pack and the energy density of the power battery. Detailed implementation manners

[0061] The present invention will be further described below in conjunction with embodiments.

[0062] General embodiment

[0063] Application of an alkenyl heptaphenyl POSS in the preparation of an injectable ceramicizable silicone heat insulation material. The structural formula of the alkenyl heptaphenyl POSS is shown as follows:

[0064]

[0065] Among them, n = 0 - 9, and more preferably 3 - 6.

[0066] The above-mentioned application of alkenyl heptaphenyl POSS in improving the injection molding process adaptability of ceramicizable silicone heat insulation materials.

[0067] Preferably, the preparation route of the alkenyl heptaphenyl POSS is as follows:

[0068]

[0069] The preparation method includes: adding an organic solvent, sodium hydroxide and water to a reactor and stirring evenly, dropping phenyltriethoxysilane, heating to reflux after dropping, and reacting; after cooling, the organic solvent is removed under vacuum, adding another organic solvent to dissolve, cooling to -5 to 0 °C, adding pyridine, and dropping an alkenyl trichlorosilane with a carbon chain length of 2 - 11 for reaction, and heating to continue the reaction to obtain alkenyl heptaphenyl POSS.

[0070] An injectable ceramicizable silicone heat insulation material of alkenyl heptaphenyl POSS is obtained by uniformly mixing components including a component A and a component B with a mass ratio of 1.5 - 2.5:1 and then heating and curing; wherein:

[0071] Component A includes raw materials in the following mass percentages: hydrogen-containing silicone oil (hydrogen content is 0.1 - 2.0 wt%) 20 - 50%, silica aerogel 5 - 25%, cobalt-zinc ferrite complex 5 - 25%, hollow glass microspheres 5 - 20%, reaction rate regulator (preferably composed of butyl succinic anhydride and 3,5-propyl-1-butyn-3-ol with an excess of alcohol, and more preferably 1:1.05 - 1.2) 0 - 1%.

[0072] Component B comprises raw materials in the following mass percentages: 20-45% of a phenyl silicone resin with low molecular weight and alkenyl groups pendant on the side chains, 5-15% of terminal alkenyl heptaphenyl POSS, 5-25% of silica aerogel, 5-25% of spherical alumina, 15-25% of a cobalt-zinc ferrite composite, 1-5% of a dispersion promoter (preferably isopropoxy tris(p-aminophenoxy) titanate), and 0.1-0.3% of a catalyst (preferably a platinum catalyst).

[0073] Preferably, the structural formula of the phenyl silicone resin with low molecular weight and alkenyl groups pendant on the side chains is as follows:

[0074]

[0075] Wherein, X is 4-10.

[0076] The synthesis route of the above-mentioned phenyl silicone resin with low molecular weight and alkenyl groups pendant on the side chains is as follows:

[0077]

[0078] Its preparation method includes: under an inert gas atmosphere with a water content of 0.05-0.1 wt%, mixing methylphenyldichlorosilane, methylvinyldichlorosilane, and diphenyldiethoxysilane evenly, and dropping them into a reaction system with an ice-salt bath, controlling the temperature at -25 to -15 °C. After the dropping is completed, continuously react for 4-8 h, during which the generated HCl is separated, the inert gas is removed, the temperature is raised to room temperature, and after continuing to react for 4-8 h, trimethylchlorosilane is dropped for end-capping reaction. After the dropping is completed, the temperature is raised to 70-90 °C, and after continuing to react for 10-15 h, low-boiling substances are removed by vacuum distillation, and then the temperature is raised to 140-160 °C for structure rearrangement for 20-30 h to obtain the phenyl silicone resin with low molecular weight and alkenyl groups pendant on the side chains. Among them, the molar ratio of methylphenyldichlorosilane, methylvinyldichlorosilane, diphenyldiethoxysilane, and trimethylchlorosilane is (0.7-0.9):(0.1-0.3):(0.8-1.2):(0.1-0.3).

[0079] Preferably, the cobalt-zinc ferrite composite is CoZnFe 4 O 8 , and its preparation reaction formula is: 4Fe(NO 3 ) 3 +Co(NO 3 ) 2 +7O 2 +Zn(NO 3 ) 2 +6C 6 H 8 O 7 →COZnFe 4 O 8+8N 2 +36CO 2 +24H 2 O. The preparation method specifically includes: fully dissolving ferric nitrate, cobalt nitrate, zinc nitrate, and citric acid in water, heating to 85 - 95 °C, reacting under the bubbling action of a continuous air stream, continuously replenishing water, filtering, and drying to obtain a cobalt-zinc ferrite composite.

[0080] A preparation method of an injectable ceramizable silicone heat insulation material based on terminal alkenyl heptaphenyl POSS, comprising the following steps:

[0081] S1: Preparation of component A: Mix and stir evenly for 1 - 3 h hydrogen-containing silicone oil, silica aerogel, cobalt-zinc ferrite composite, hollow glass microspheres, and reaction rate regulator under the conditions of a temperature below 40 °C and a vacuum of -0.01 to -0.1 Mpa to obtain component A.

[0082] S2: Preparation of component B: Mix and stir evenly for 1 - 3 h phenyl silicone resin with low molecular weight side-chain pendant alkenyl groups, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt-zinc ferrite composite, dispersion promoter, and catalyst under the conditions of a temperature below 60 °C and a vacuum of -0.01 to -0.1 Mpa to obtain component B.

[0083] S3: Mix component A and component B evenly, heat to 50 - 90 °C for curing, and complete the curing within 3 min.

[0084] Raw material preparation Example 1: Preparation of vinyl heptaphenyl POSS

[0085] Add 200 mL of tetrahydrofuran, 2.8 g (0.07 mol) of sodium hydroxide, and 3.34 g of secondary distilled water to a 500 mL three-necked flask equipped with a condenser and a stirrer. After stirring evenly, slowly dropwise add 30.66 g (0.13 mol) of phenyltriethoxysilane. After dropping, heat to reflux and react for 5 h. After cooling to room temperature, remove tetrahydrofuran under vacuum, and add 100 mL of methanol for dissolution. After complete dissolution, cool to 0 °C, add 4.4 g of pyridine, dropwise add 3.0 g (0.0186 mol) of vinyltrichlorosilane, react for 12 h, then rise to room temperature and continue to react for 12 h. Filter, wash with methanol, and remove the solvent to obtain 18.2 g of vinyl heptaphenyl cage-like silsesquioxane (vinyl heptaphenyl POSS). The preparation route is as follows:

[0086]

[0087] Among them, n = 0.

[0088] Raw material preparation Example 2: Preparation of octenyl heptaphenyl POSS

[0089] In a 500 mL three-necked flask equipped with a condenser and a stirrer, 200 mL of tetrahydrofuran, 2.8 g (0.07 mol) of sodium hydroxide, and 3.34 g of secondary distilled water were added. After stirring evenly, 30.66 g (0.13 mol) of phenyltriethoxysilane was slowly added dropwise. After the addition was complete, the mixture was heated to reflux and reacted for 5 h. After cooling to room temperature, tetrahydrofuran was removed under vacuum, and 100 mL of methanol was added to dissolve. After complete dissolution, the temperature was lowered to 0 °C, 4.4 g of pyridine was added, and 4.57 g (0.0186 mol) of octenyltrichlorosilane was added dropwise. After reacting for 12 h, the temperature was raised to room temperature and the reaction continued for 12 h. After filtration and washing with methanol, the solvent was removed to obtain 19.6 g of octenyl heptaphenylcage silsesquioxane (octenyl heptaphenyl POSS). The preparation route is as follows:

[0090]

[0091] Among them, n = 6.

[0092] Raw material preparation example 3: Preparation of undecenyl heptaphenyl POSS

[0093] In a 500 mL three-necked flask equipped with a condenser and a stirrer, 200 mL of tetrahydrofuran, 2.8 g (0.07 mol) of sodium hydroxide, and 3.34 g of secondary distilled water were added. After stirring evenly, 30.66 g (0.13 mol) of phenyltriethoxysilane was slowly added dropwise. After the addition was complete, the mixture was heated to reflux and reacted for 5 h. After cooling to room temperature, tetrahydrofuran was removed under vacuum, and 100 mL of methanol was added to dissolve. After complete dissolution, the temperature was lowered to 0 °C, 4.4 g of pyridine was added, and 5.35 g (0.0186 mol) of undecenyltrichlorosilane was added dropwise. After reacting for 12 h, the temperature was raised to room temperature and the reaction continued for 12 h. After filtration and washing with methanol, the solvent was removed to obtain 20.2 g of n-octenyl heptaphenylcage silsesquioxane (undecenyl heptaphenyl POSS). The preparation route is as follows:

[0094]

[0095] Among them, n = 9.

[0096] Raw material preparation example 4: Preparation of cobalt-zinc ferrite composite

[0097] Ferric nitrate (96.7 g, 0.4 mol), cobalt nitrate (18.3 g, 0.1 mol), zinc nitrate (18.9 g, 0.1 mol), and citric acid (115.3 g, 0.6 mol) were fully dissolved in secondary distilled water, heated to 90 °C, and under the bubbling action of a continuous air stream, and secondary distilled water was continuously replenished. The reaction was carried out for 24 h. After filtration and vacuum drying, a cobalt-zinc ferrite composite was obtained with a yield of 99.8%. The reaction formula is as follows: 4Fe(NO 3 )3 +Co(NO 3 ) 2 +7O 2 +Zn(NO 3 ) 2 +6C 6 H 8 O 7 →CoZnFe 4 O 8 +8N 2 +36CO 2 +24H 2 O

[0098] Example 5 of raw material preparation: Preparation of phenyl silicone resin with low molecular weight side chain pendant alkenyl

[0099] Under the protection of nitrogen with a water content of 0.1 wt%, methylphenyldichlorosilane (152.8 g, 0.8 mol), methylvinyldichlorosilane (28.2 g, 0.2 mol), and diphenyldiethoxysilane (272.4 g, 1 mol) were mixed evenly and added dropwise to a reaction system with an ice-salt bath. The temperature was controlled at -18 °C. After the addition was completed, the generated HCl was filtered off by a vacuum device. After 6 h of continuous reaction, the filtration device was removed, the inert gas was removed, and the temperature was raised to room temperature. After continuing the reaction for 6 h, trimethylchlorosilane (21.8 g, 0.2 mol) was slowly added dropwise for end-capping reaction. After the addition was completed, the temperature was raised to 80 °C. After continuing the reaction for 12 h, low-boiling substances were removed by vacuum distillation, and then the temperature was raised to 150 °C for 24 h of structure rearrangement to obtain phenyl silicone resin with low molecular weight side chain pendant alkenyl.

[0100] The product was tested by GPC, with Mn being 3654, Mw being 6943, and the dispersity being 1.90. Tested by a rotational viscometer, the viscosity of the system was 1.54 Pa·S. The preparation route is as follows:

[0101]

[0102] Example of preparation of silicone thermal insulation material:

[0103] It was obtained by uniformly mixing component A and component B in a weight ratio of 2:1 and curing by heating.

[0104] The specific formula of component A is as follows: hydrogen-containing silicone oil 20 - 50 wt%, silica aerogel 5 - 25 wt%, cobalt-zinc ferrite complex 5 - 25 wt%, hollow glass microspheres 5 - 20 wt%, reaction rate regulator 0 - 1 wt%.

[0105] Among them, the hydrogen-containing silicone oil is provided by Guangdong Chenxi New Materials Technology Co., Ltd., the silica aerogel is provided by Gongyi Fanrui Yihui Composite Materials Co., Ltd., the cobalt-zinc ferrite composite is prepared according to Preparation Example 4 of the raw materials, the hollow glass microspheres are provided by Shanxi Hainuo Technology Co., Ltd., and the reaction rate regulator is a mixture of butyl succinic anhydride and 3,5-propyl-1-butyne-3-ol in a molar ratio of 1:1.1.

[0106] Preparation of Component A (A1): Add 45.5 parts of hydrogen-containing silicone oil (hydrogen content 0.18%), 19 parts of silica aerogel, 20 parts of cobalt-zinc ferrite composite, 15 parts of hollow glass microspheres, and 0.5 part of reaction rate regulator to a high-speed dispersion planetary mixer, control the temperature below 40°C, mix and stir for 2 h, with a vacuum degree of -0.1 Mpa. After stirring evenly, discharge to obtain Component A (A1).

[0107] Preparation of Component A (A2): Add 40.5 parts of hydrogen-containing silicone oil (hydrogen content 0.8%), 19 parts of silica aerogel, 25 parts of cobalt-zinc ferrite composite, 15 parts of hollow glass microspheres, and 0.5 part of reaction rate regulator to a high-speed dispersion planetary mixer, control the temperature below 40°C, mix and stir for 2 h, with a vacuum degree of -0.1 Mpa. After stirring evenly, discharge to obtain Component A (A2).

[0108] Preparation of Component A (A3): Add 35 parts of hydrogen-containing silicone oil (hydrogen content 1.5%), 19 parts of silica aerogel, 25 parts of cobalt-zinc ferrite composite, 20 parts of hollow glass microspheres, and 1 part of reaction rate regulator to a high-speed dispersion planetary mixer, control the temperature below 40°C, mix and stir for 2 h, with a vacuum degree of -0.1 Mpa. After stirring evenly, discharge to obtain Component A (A3).

[0109] The specific formulation of Component B is as follows: 20 - 45 wt% of phenyl silicone resin with low molecular weight and pendant alkenyl groups on the side chain, 5 - 15 wt% of terminal alkenyl heptaphenyl POSS, 5 - 25 wt% of silica aerogel, 5 - 25 wt% of spherical alumina, 15 - 25 wt% of cobalt-zinc ferrite composite, 1 - 5 wt% of dispersion promoter, and 0.1 - 0.3 wt% of platinum catalyst.

[0110] Among them, the phenyl silicone resin with low molecular weight and pendant alkenyl groups on the side chain is prepared according to Preparation Example 5 of the raw materials, the terminal alkenyl heptaphenyl POSS is prepared according to Preparation Examples 1 - 3 of the raw materials, the silica aerogel is provided by Gongyi Fanrui Yihui Composite Materials Co., Ltd., the spherical alumina is provided by Zibo Qimingxing New Materials Co., Ltd., the cobalt-zinc ferrite composite is prepared according to Preparation Example 4 of the raw materials, the dispersion promoter is isopropoxy tris(p-aminophenoxy) titanate, and the platinum catalyst is KARSTEDT catalyst.

[0111] Preparation of Component B (B1): Add 40 parts of phenyl silicone resin with low molecular weight and vinyl side chains, 15 parts of vinyl heptaphenyl POSS (Example 1), 18 parts of silica aerogel, 5 parts of spherical alumina, 17 parts of cobalt-zinc ferrite composite, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst into a high-speed dispersion planetary mixer. Control the temperature below 60°C and mix and stir for 2 h with a vacuum of -0.1 Mpa. After stirring evenly, discharge to obtain Component B (B1).

[0112] Preparation of Component B (B2): Add 35 parts of phenyl silicone resin with low molecular weight and vinyl side chains, 10 parts of vinyl heptaphenyl POSS (Example 1), 13 parts of silica aerogel, 21 parts of spherical alumina, 16 parts of cobalt-zinc ferrite composite, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst into a high-speed dispersion planetary mixer. Control the temperature below 60°C and mix and stir for 2 h with a vacuum of -0.1 Mpa. After stirring evenly, discharge to obtain Component B (B2).

[0113] Preparation of Component B (B3): Add 30 parts of phenyl silicone resin with low molecular weight and vinyl side chains, 5 parts of vinyl heptaphenyl POSS (Example 1), 13 parts of silica aerogel, 25 parts of spherical alumina, 22 parts of cobalt-zinc ferrite composite, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst into a high-speed dispersion planetary mixer. Control the temperature below 60°C and mix and stir for 2 h with a vacuum of -0.1 Mpa. After stirring evenly, discharge to obtain Component B (B3).

[0114] Preparation of Component B (B4): Add 30 parts of phenyl silicone resin with low molecular weight and vinyl side chains, 5 parts of octenyl heptaphenyl POSS (Example 2), 13 parts of silica aerogel, 25 parts of spherical alumina, 22 parts of cobalt-zinc ferrite composite, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst into a high-speed dispersion planetary mixer. Control the temperature below 60°C and mix and stir for 2 h with a vacuum of -0.1 Mpa. After stirring evenly, discharge to obtain Component B (B4).

[0115] Preparation of Component B (B5): Add 30 parts of phenyl silicone resin with low molecular weight and vinyl side chains, 5 parts of undecenyl heptaphenyl POSS (Example 3), 13 parts of silica aerogel, 25 parts of spherical alumina, 22 parts of cobalt-zinc ferrite composite, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst into a high-speed dispersion planetary mixer. Control the temperature below 60°C and mix and stir for 2 h with a vacuum of -0.1 Mpa. After stirring evenly, discharge to obtain Component B (B5).

[0116] After mixing the A and B components evenly at a ratio of 2:1, the viscosity is relatively low, making it suitable for injection molding. Heat it to 80 °C and complete the curing within 3 minutes.

[0117] Curing Examples

[0118] Curing Example 1: A1 + B1;

[0119] Curing Example 2: A2 + B2;

[0120] Curing Example 3: A3 + B3;

[0121] Curing Example 4: A3 + B4;

[0122] Curing Example 5: A3 + B5.

[0123] Comparative Examples

[0124] Comparative Example 1: Compared with Curing Example 3, the difference is that the B component does not contain terminal alkenyl heptaphenyl POSS, and is replaced with a phenyl silicone resin with low molecular weight side chain suspended alkenyl of equal mass.

[0125] The formula of the B component (B6) is: 35 parts of phenyl silicone resin with low molecular weight side chain suspended alkenyl, 13 parts of silica aerogel, 25 parts of spherical alumina, 22 parts of cobalt zinc ferrite complex, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst.

[0126] Comparative Example 2: Compared with Curing Example 3, the difference is that the B component (B7) uses a phenyl silicone resin with high molecular weight side chain suspended alkenyl of equal mass, and the average molecular weight Mn of the phenyl silicone resin with high molecular weight side chain suspended alkenyl is 100,000.

[0127] Comparative Example 3: Compared with Curing Example 3, the difference is that the A and B components do not contain cobalt zinc ferrite complex, and are replaced with silica aerogel, hollow glass microspheres and spherical alumina.

[0128] The formula of the A component (A4) is: 35 parts of hydrogen-containing silicone oil (hydrogen content 1.5%), 29 parts of silica aerogel, 35 parts of hollow glass microspheres, and 1 part of reaction rate regulator.

[0129] The formula of the B component (B8) is: 30 parts of phenyl silicone resin with low molecular weight side chain suspended alkenyl, 5 parts of vinyl heptaphenyl POSS (Example 1), 20 parts of silica aerogel, 40 parts of spherical alumina, 4.9 parts of dispersion promoter, and 0.1 part of KARSTEDT catalyst.

[0130] Performance Test

[0131] The silicone thermal insulation materials obtained by mixing and heating different A components and B components for curing were subjected to performance tests, and the data are shown in the following table:

[0132]

[0133]

[0134] *1 The method for measuring the temperature on the back side of the coating is the temperature measured on the back side after continuously spraying and burning the front side of the 0.3-mm coating with the above high-temperature flame for 30 minutes. The viscosity before curing is measured by sampling after the A and B components are evenly mixed.

[0135] *2 The commercially available comparative example is a silicone heat-insulating and insulating coating prepared by a commercially available molding technique (provided by Ningbo Juli Company).

[0136] It can be seen from the data comparison in the above table that:

[0137] In terms of the viscosity of the mixture before curing, the viscosities of Curing Examples 1-5 of the present invention are lower than those of Comparative Examples 1 and 2. Therefore, it is very suitable for the injection molding process. The reason is that the difference between Comparative Example 1 and Curing Example 3 is that in the B component, phenyl silicone resin with low molecular weight and side-chain-suspended alkenyl is replaced with an equal mass. Due to the lack of the viscosity-reducing effect of phenyl POSS, the viscosity of the material increases; the difference between Comparative Example 2 and Curing Example 3 is that in the B component, phenyl silicone resin with high molecular weight and side-chain-suspended alkenyl is used to replace phenyl silicone resin with low molecular weight and side-chain-suspended alkenyl. The too high molecular weight leads to an increase in the viscosity of the system. By comparing Curing Examples 3-5, it can be found that the viscosity of Curing Example 4 is slightly higher than that of Curing Example 3. The reason is that octenyl heptaphenyl POSS is added in Curing Example 4, and the viscosity will slightly increase compared with vinyl heptaphenyl POSS added in Curing Example 3. However, the vinyl carbon chain length of vinyl heptaphenyl POSS is short, and due to steric hindrance, the participation rate of the addition reaction is low, resulting in a decrease in the crosslinking density, making the tensile strength of the cured material significantly inferior to that of Curing Example 4; in addition, it can be found that the viscosity of Curing Example 5 is significantly higher than that of Curing Example 3. This is because undecenyl heptaphenyl POSS is added in Curing Example 5, and the alkenyl carbon chain length of undecenyl heptaphenyl POSS is long, which increases the viscosity of the system to a certain extent. In addition, compared with Curing Examples 1-5, the commercially available products of the commercially available comparative example cannot be injection molded and can only be processed by the molding process, and the curing time needs to be greater than 20 minutes. While Curing Examples 1-5 only need ≤5 minutes, and the curing time is short.

[0138] In addition, in terms of tensile strength, heat insulation and heat resistance, it can also be found that Curing Examples 1-5 are significantly superior to each comparative example.

[0139] The raw materials and equipment used in the present invention, unless otherwise specified, are all common raw materials and equipment in the art; the methods used in the present invention, unless otherwise specified, are all conventional methods in the art.

[0140] The above are only the preferred embodiments of the present invention and do not impose any limitations on the present invention. Any simple modifications, changes, and equivalent transformations made to the above embodiments based on the technical essence of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims

1. Application of terminal alkenyl heptaphenyl POSS in preparing injectable ceramizable silicone heat insulation materials, Characterized in that: The structural formula of terminal alkenyl heptaphenyl POSS is as follows: Wherein, n = 3 - 6; The injectable ceramizable silicone heat insulation material is obtained by uniformly mixing components including component A and component B and heating and curing; Component A includes: hydrogen-containing silicone oil, silica aerogel, cobalt zinc ferrite complex, hollow glass microspheres, reaction rate regulator; Component B includes: low molecular weight phenyl silicone resin with pendant alkenyl side chains, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter, catalyst.

2. Application of terminal alkenyl heptaphenyl POSS in improving the injection molding process adaptability of ceramizable silicone heat insulation materials, Characterized in that: The structural formula of terminal alkenyl heptaphenyl POSS is as follows: Wherein, n = 3 - 6; The injectable ceramizable silicone heat insulation material is obtained by uniformly mixing components including component A and component B and heating and curing; Component A includes: hydrogen-containing silicone oil, silica aerogel, cobalt zinc ferrite complex, hollow glass microspheres, reaction rate regulator; Component B includes: low molecular weight phenyl silicone resin with pendant alkenyl side chains, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter, catalyst.

3. The application according to claim 1 or 2, Characterized in that: The preparation route of the terminal alkenyl heptaphenyl POSS is:

4. The application according to claim 3, Characterized in that: The preparation method of the terminal alkenyl heptaphenyl POSS includes: adding an organic solvent, sodium hydroxide and water into a reactor and stirring evenly, dropping phenyltriethoxysilane, heating to reflux after dropping, and reacting; after cooling, the organic solvent is removed under vacuum, adding another organic solvent to dissolve, cooling to -5 to 0 °C, adding pyridine, dropping terminal alkenyl trichlorosilane with a carbon chain length of 2 - 11 for reaction, and heating to continue the reaction to obtain terminal alkenyl heptaphenyl POSS.

5. An injectable ceramizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS, Characterized in that: It is obtained by uniformly mixing components including component A and component B and heating and curing; wherein: Component A includes the following raw materials: hydrogen-containing silicone oil, silica aerogel, cobalt zinc ferrite complex, hollow glass microspheres, reaction rate regulator; Component B includes the following raw materials: low molecular weight phenyl silicone resin with pendant alkenyl side chains, terminal alkenyl heptaphenyl POSS in the application according to any one of claims 1 - 4, silica aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter, catalyst.

6. The injectable ceramizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS according to claim 5, Characterized in that: Component A includes the following raw materials in mass percentages: hydrogen-containing silicone oil 20 - 50%, silica aerogel 5 - 25%, cobalt zinc ferrite complex 5 - 25%, hollow glass microspheres 5 - 20%, reaction rate regulator 0 - 1%; The second component includes raw materials in the following mass percentages: 20-45% of phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups, 5-15% of terminal alkenyl heptaphenyl POSS, 5-25% of silica aerogel, 5-25% of spherical alumina, 15-25% of cobalt zinc ferrite complex, 1-5% of dispersion promoter, and 0.1-0.3% of catalyst.

7. The injectable ceramicizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS according to claim 5 or 6, characterized in that: The structural formula of the phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups is as follows: wherein, X is 4-10; and / or The cobalt-zinc ferrite composite is CoZnFe 4 O 8 .

8. A preparation method of the injectable ceramicizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS according to any one of claims 5-7, characterized in that it includes the following steps: S1: Preparation of the first component: Mix hydrogen-containing silicone oil, silica aerogel, cobalt zinc ferrite complex, hollow glass microspheres, and reaction rate regulator evenly to obtain the first component; S2: Preparation of the second component: Mix phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter, and catalyst evenly to obtain the second component; S3: Mix the first component and the second component evenly and cure by heating.

9. The preparation method according to claim 8, characterized in that: In S1, mix hydrogen-containing silicone oil, silica aerogel, cobalt zinc ferrite complex, hollow glass microspheres, and reaction rate regulator evenly under the conditions of a temperature lower than 40°C and a vacuum degree of -0.01 to -0.1 Mpa to obtain the first component; In S2, mix phenyl silicone resin with low molecular weight and side-chain pendant alkenyl groups, terminal alkenyl heptaphenyl POSS, silica aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter, and catalyst evenly under the conditions of a temperature lower than 60°C and a vacuum degree of -0.01 to -0.1 Mpa to obtain the second component; In S3, mix the first component and the second component evenly and heat to 50-90°C for curing.

10. An injectable ceramicizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS according to any one of claims 5-7 or an injectable ceramicizable silicone heat insulation material of terminal alkenyl heptaphenyl POSS obtained by the preparation method according to claim 8 or 9, characterized in that: The viscosity of the injectable ceramicizable silicone heat insulation material before curing is ≤25 Pa·S, the curing time is ≤5 min, and the tensile strength after curing and molding is ≥1.7 MPa.

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