Two-component silicone structural sealant and method for producing the same
By using temperature-reactive phase change microcapsules to release highly active titanium-based co-catalysts at low temperatures, the problem of slow curing speed and low crosslinking density of two-component silicone structural sealants at low temperatures is solved, achieving rapid curing and high-performance bonding in low-temperature environments.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIANGXI LEDIA ENERGY SAVING TECH CO LTD
- Filing Date
- 2026-05-09
- Publication Date
- 2026-06-12
AI Technical Summary
Existing two-component silicone structural sealants have slow curing speed and low crosslinking density in low-temperature environments of ≤5℃, resulting in permanent deficiencies in bond strength and elastic recovery rate, which cannot meet construction requirements.
A highly active titanium-based cocatalyst is encapsulated in temperature-reactive phase change microcapsules. The core-shell structure of the temperature-reactive phase change microcapsules ruptures at ≤5℃ to release the highly active titanium-based cocatalyst. Combined with a low-activity organic bismuth catalyst, low-temperature synergistic catalysis is achieved, which improves the rate and density of crosslinking reaction.
It accelerates curing speed, increases crosslinking density, improves bonding strength and elastic recovery rate in low-temperature environments of ≤5℃, and meets construction performance requirements.
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Figure CN122188577A_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the field of silicone structural sealant technology, and particularly relates to a two-component silicone structural sealant and its preparation method. Background Technology
[0002] Two-component silicone structural sealant is an adhesive material used in building curtain wall engineering. It mainly consists of a base component and a curing agent component. When used, it is mixed according to the ratio and then cross-linked and cured through a condensation reaction. It has excellent weather resistance, long-term elastic recovery ability and stable adhesion to multiple substrates. It is a key material for transferring structural loads and ensuring the long-term safety of buildings in structural bonding systems such as frameless glass curtain walls. It is also widely used in structural bonding and long-term sealing scenarios in industrial equipment, rail transit, new energy facilities and other fields.
[0003] However, existing two-component silicone structural sealants suffer from slow curing speed and low crosslinking density in low-temperature construction scenarios (≤5℃), leading to permanent deficiencies in bond strength and elastic recovery. Specifically, the conventional condensation curing system used in existing two-component silicone structural sealants has inherent performance defects in the ≤5℃ low-temperature range: the catalyst used to drive the crosslinking reaction experiences a sharp drop in catalytic activity at ≤5℃, and the low-temperature environment significantly reduces the mobility and reaction efficiency of the base resin molecular chains. These two factors combined result in the product failing to achieve uniform and complete qualified curing. In scenarios requiring construction operations at ≤5℃, such as outdoor curtain wall construction in northern my country during winter, emergency bonding of infrastructure projects in cold regions, and emergency repair of existing building curtain walls damaged in winter, existing products cannot achieve the qualified performance indicators required for structural bonding after construction, failing to guarantee the long-term safety of the structural system. Therefore, industry standards have imposed strict restrictions on such construction operations in ≤5℃ low-temperature environments. Summary of the Invention
[0004] The purpose of this application is to provide a two-component silicone structural sealant and its preparation method, which can improve the defects of two-component silicone structural sealant in low temperature construction environment ≤5℃, such as slow curing speed and low crosslinking density, which leads to permanent insufficient bonding strength and elastic recovery rate.
[0005] To achieve the above-mentioned objectives, the technical solution adopted in this application is as follows: In a first aspect, this application provides a two-component silicone structural sealant, comprising component A and component B; wherein... Component A comprises the following components in parts by weight: α,ω-dihydroxypolydimethylsiloxane, 90-110 parts; Reinforcing filler, 10-20 parts; Composite silane coupling agent, 1-3 parts; Component B comprises the following components in parts by weight: Silane crosslinking agent, 55-65 parts; Low-activity organic bismuth catalyst, 1-3 parts; Temperature-reversible phase change microcapsules, 10-20 parts; The temperature-reactive phase change microcapsule has a core-shell structure. The wall material of the temperature-reactive phase change microcapsule is a composite wall material of melamine-formaldehyde resin and polyurethane. The core material of the temperature-reactive phase change microcapsule includes n-tetradecane and a highly active titanium-based cocatalyst. The temperature-reactive phase change microcapsule can rupture and release the highly active titanium-based cocatalyst when the curing construction environment temperature is ≤5℃.
[0006] The two-component silicone structural sealant provided in this application includes component A and component B. Component A uses 90-110 parts of α,ω-dihydroxypolydimethylsiloxane as the base film-forming matrix of the two-component silicone structural sealant, providing the core elastic skeleton, weather resistance, and basic mechanical load-bearing capacity for the cured sealant; 10-20 parts of reinforcing filler significantly improve the tensile strength, tear strength, and deformation resistance of the cured sealant; 1-3 parts of composite silane coupling agent significantly improve the interfacial adhesion strength between the sealant and commonly used curtain wall substrates such as glass, aluminum alloy, and stone; component B uses 5... 5-65 parts of silane crosslinking agent undergo a condensation crosslinking reaction with α,ω-dihydroxypolydimethylsiloxane in component A to construct a three-dimensional network elastic structure, which is the core reaction component for the transformation of the colloid from a liquid paste to an elastic solid; 1-3 parts of low-activity organic bismuth catalyst can provide a smooth and stable catalytic efficiency at temperatures above 5°C, ensuring that the mixed colloid has a sufficient application period, while reducing the problems of shortened application window and decreased storage stability caused by excessively rapid crosslinking reaction at temperatures above 5°C; 10-20 parts of temperature-reactive phase change microcapsules serve as a highly active cocatalyst at temperatures below 5°C. The encapsulation and controlled release carrier achieves complete sealing and isolation at temperatures above 5°C and precise triggered release at temperatures below 5°C, providing core functional support for improved curing performance at temperatures below 5°C. The thermo-responsive phase change microcapsules have a core-shell structure, with the wall material being a composite of melamine-formaldehyde resin and polyurethane. This provides excellent toughness and shear resistance at temperatures above 5°C, withstanding high-pressure shearing during adhesive application without cracking, while also exhibiting sufficient brittleness at temperatures below 5°C, allowing for successful cracking by the stress generated by the phase change of the core material. The core material of the thermo-responsive phase change microcapsules includes n-tetradecane and highly active... The titanium-based cocatalyst can provide precise temperature triggering for the rupture of thermosensitive phase change microcapsules through the phase change characteristics of n-tetradecane. At the same time, the highly active titanium-based cocatalyst provides sufficient catalytic activity for crosslinking reactions at ≤5℃, making up for the catalytic efficiency gap at ≤5℃. The thermosensitive phase change microcapsules can rupture and release highly active titanium-based cocatalysts at ambient temperatures ≤5℃, precisely matching the temperature range that is a pain point for low-temperature construction in the industry. The release of highly active cocatalysts is triggered only at the target low-temperature environment, achieving a targeted improvement in low-temperature curing efficiency without affecting the construction and storage performance at room temperature.
[0007] This two-component silicone structural sealant maintains the integrity of the wall material of the thermo-responsive phase change microcapsules in environments above 5℃, effectively isolating and sealing the highly active titanium-based cocatalyst to prevent premature reaction and subsequent decrease in system storage stability. In construction environments below 5℃, the tetradecane phase change in the core material of the thermo-responsive phase change microcapsules causes rupture, releasing the highly active titanium-based cocatalyst. The highly active titanium-based cocatalyst and the low-activity organic bismuth catalyst form a low-temperature synergistic catalytic effect, accelerating the condensation crosslinking reaction rate between the silane crosslinking agent and α,ω-dihydroxypolydimethylsiloxane, while also ensuring a more complete crosslinking reaction. Combined with the interfacial reinforcement effect of reinforcing fillers and composite silane coupling agents, this sealant effectively improves the problems of slow curing speed and low crosslinking density in existing two-component silicone structural sealants under low-temperature construction environments below 5℃, which leads to permanent substandard bonding strength and elastic recovery rate.
[0008] Secondly, this application provides a method for preparing a two-component silicone structural sealant as described in the first aspect, applied to a sealant preparation system, the sealant preparation system including a stirring execution module and a temperature control module, the method comprising: The α,ω-dihydroxypolydimethylsiloxane, the reinforcing filler, and the composite silane coupling agent are mixed evenly to obtain component A. The silane crosslinking agent and the low-activity organic bismuth catalyst were mixed evenly to obtain the basic system of component B. The n-tetradecane and the highly active titanium-based co-catalyst are mixed evenly to obtain the core material of the temperature-reversible phase change microcapsule; The core material is coated and cured using the melamine-formaldehyde resin and polyurethane composite wall material to obtain the temperature-reversible phase change microcapsules. The inverse temperature response phase change microcapsules are added to the B-component base system, stirred and dispersed, and the shear stress and temperature information of the B-component base system are obtained; wherein, the shear stress information is used to reflect the magnitude of the shear impact on the inverse temperature response phase change microcapsules during the dispersion process, and the temperature information is used to reflect the temperature fluctuation of the B-component base system during the dispersion process. The rotation speed of the stirring execution module is controlled based on the shear stress information, and the output power of the temperature control module is controlled based on the temperature information to obtain the uniformly dispersed component B. The A component and the B component are sealed and stored separately to obtain the two-component silicone structural sealant.
[0009] The method for preparing the two-component silicone structural sealant provided in this application involves uniformly mixing α,ω-dihydroxypolydimethylsiloxane, reinforcing filler, and composite silane coupling agent to obtain component A. This method ensures uniform dispersion of the reinforcing filler in the base adhesive, providing a stable foundation for the mechanical strength and adhesive properties of component A. Uniformly mixing the silane crosslinking agent with a low-activity organic bismuth catalyst yields component B, preventing premature deactivation of the low-activity organic bismuth catalyst and ensuring the room-temperature storage stability of component B. Uniformly mixing n-tetradecane with a highly active titanium-based co-catalyst yields the core material for thermo-responsive phase change microcapsules, providing temperature-response triggering and low-temperature curing catalysis functions. Encapsulating and curing the core material with a melamine-formaldehyde resin and polyurethane composite wall material yields the thermo-responsive phase change microcapsules, enabling the isolation and encapsulation of the highly active titanium-based co-catalyst at temperatures above 5°C, preventing the highly active titanium-based co-catalyst from interacting with the component B base. The process involves an early reaction, ensuring the wall material possesses controllable temperature-responsive encapsulation breaking performance. Adding inverse temperature-responsive phase change microcapsules to the B-component base system, followed by stirring and dispersion, and obtaining shear stress and temperature information for the B-component base system, enables uniform dispersion of the microcapsules within the B-component base system, providing reliable data for subsequent precise process control. Controlling the stirring speed based on shear stress information and the output power of the temperature control module based on temperature information results in uniformly dispersed B-component. This ensures uniform dispersion of the inverse temperature-responsive phase change microcapsules while reducing premature encapsulation caused by shear impact and minimizing the impact of temperature fluctuations on wall material stability, balancing dispersion effectiveness with the structural integrity of the microcapsules. Separating and storing components A and B independently yields a two-component silicone structural sealant, which isolates cross-linking reaction components, ensuring product performance stability during storage and preventing premature curing and failure. The two-component silicone structural sealant prepared by this method can improve the existing two-component silicone structural sealant, which has the defects of slow curing speed and low crosslinking density in low temperature environment ≤5℃, resulting in permanent insufficient bonding strength and elastic recovery rate.
[0010] The above description is only an overview of the technical solution of this application. In order to better understand the technical means of this application and to implement it in accordance with the contents of the specification, and to make the above and other objects, features and advantages of this application more obvious and understandable, the following are specific embodiments of this application. Attached Figure Description
[0011] To more clearly illustrate the technical solutions in the embodiments of this application, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0012] Figure 1 This is a schematic flowchart of the preparation method of the two-component silicone structural sealant provided in the embodiments of this application; Figure 2 This is a schematic diagram of the first part of the implementation process of step S600 in the preparation method of the two-component silicone structural sealant provided in the embodiments of this application; Figure 3 This is a schematic diagram of the implementation process of step S613 in the preparation method of the two-component silicone structural sealant provided in the embodiments of this application; Figure 4 This is a schematic diagram of the second part of the implementation process of step S600 in the preparation method of the two-component silicone structural sealant provided in the embodiments of this application; Figure 5 This is a schematic diagram of the implementation process of step S621 in the preparation method of the two-component silicone structural sealant provided in the embodiments of this application. Detailed Implementation
[0013] To make the technical problems, technical solutions, and beneficial effects of this application clearer, the following detailed description is provided in conjunction with embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.
[0014] In this application, the term "and / or" describes the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. A and B can be singular or plural. The character " / " generally indicates that the preceding and following related objects have an "or" relationship.
[0015] In this application, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or multiple items. For example, "at least one of a, b, or c", or "at least one of a, b, and c", can both mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple.
[0016] It should be understood that in the various embodiments of this application, the order of the above processes does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.
[0017] The terminology used in the embodiments of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of this application. The singular forms “a,” “the,” and “the” used in the embodiments of this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.
[0018] The weights of the relevant components mentioned in the embodiments of this application can refer not only to the specific content of each component, but also to the proportional relationship between the weights of the components. Therefore, any scaling up or down of the content of the relevant components according to the embodiments of this application is within the scope disclosed in the embodiments of this application. Specifically, the mass described in the embodiments of this application can be a well-known unit of mass in the chemical industry, such as µg, mg, g, or kg.
[0019] The terms "first" and "second" are used for descriptive purposes only, to distinguish objects, such as substances, from one another, and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. For example, without departing from the scope of the embodiments of this application, "first XX" may also be referred to as "second XX," and similarly, "second XX" may also be referred to as "first XX." Thus, features defined with "first" and "second" may explicitly or implicitly include one or more of that feature.
[0020] Two-component silicone structural sealant is an adhesive material used in building curtain wall engineering. It mainly consists of a base component and a curing agent component. When used, it is mixed according to the ratio and then cross-linked and cured through a condensation reaction. It has excellent weather resistance, long-term elastic recovery ability and stable adhesion to multiple substrates. It is a key material for transferring structural loads and ensuring the long-term safety of buildings in structural bonding systems such as frameless glass curtain walls. It is also widely used in structural bonding and long-term sealing scenarios in industrial equipment, rail transit, new energy facilities and other fields.
[0021] However, existing two-component silicone structural sealants suffer from slow curing speed and low crosslinking density in low-temperature construction scenarios (≤5℃), leading to permanent deficiencies in bond strength and elastic recovery. Specifically, the conventional condensation curing system used in existing two-component silicone structural sealants has inherent performance defects in the ≤5℃ low-temperature range: the catalyst used to drive the crosslinking reaction experiences a sharp drop in catalytic activity at ≤5℃, and the low-temperature environment significantly reduces the mobility and reaction efficiency of the base resin molecular chains. These two factors combined result in the product failing to achieve uniform and complete qualified curing. In scenarios requiring construction operations at ≤5℃, such as outdoor curtain wall construction in northern my country during winter, emergency bonding of infrastructure projects in cold regions, and emergency repair of existing building curtain walls damaged in winter, existing products cannot achieve the qualified performance indicators required for structural bonding after construction, failing to guarantee the long-term safety of the structural system. Therefore, industry standards have imposed strict restrictions on such construction operations in ≤5℃ low-temperature environments.
[0022] Based on this, in order to improve the defects of two-component silicone structural sealants in related technologies, which have slow curing speed and low crosslinking density in low temperature construction environment of ≤5℃, resulting in permanent insufficient bonding strength and elastic recovery rate, the embodiments of this application provide the following solutions.
[0023] The first aspect of this application provides a two-component silicone structural sealant, comprising component A and component B. Component A comprises the following components by weight: α,ω-dihydroxypolydimethylsiloxane, 90-110 parts; reinforcing filler, 10-20 parts; composite silane coupling agent, 1-3 parts. Component B comprises the following components by weight: silane crosslinking agent, 55-65 parts; low-activity organic bismuth catalyst, 1-3 parts; and thermo-responsive phase change microcapsules, 10-20 parts. The thermo-responsive phase change microcapsules have a core-shell structure, and the wall material of the microcapsules is a melamine-formaldehyde resin and polyurethane composite wall material. The core material of the thermo-responsive phase change microcapsules includes n-tetradecane and a highly active titanium-based co-catalyst. The thermo-responsive phase change microcapsules can rupture and release the highly active titanium-based co-catalyst when the curing construction environment temperature is ≤5℃.
[0024] It is understood that α,ω-dihydroxy polydimethylsiloxane is the base polymer of two-component silicone structural sealants. Its molecular chains have hydroxyl functional groups at both ends, which can undergo condensation reactions with silane crosslinking agents to form a three-dimensional crosslinked network. Reinforcing fillers are inorganic fillers that can improve the mechanical strength of two-component silicone structural sealants; for example, they can be one or more of surface-modified nano-calcium carbonate, fumed silica, and precipitated silica. Composite silane coupling agents are mixtures of two or more silane coupling agents used to improve the interfacial compatibility between reinforcing fillers and the base polymer, thereby enhancing adhesion performance. Silane crosslinking agents are silane compounds containing three or more hydrolyzable alkoxy groups, such as one or more of methyltrimethoxysilane, methyltriethoxysilane, and vinyltrimethoxysilane, which can undergo condensation reactions with the hydroxyl groups of α,ω-dihydroxy polydimethylsiloxane to achieve crosslinking and curing.
[0025] Low-activity organobismuth catalysts are organobismuth compounds with milder catalytic activity and greater stability at room temperature in two-component silicone structural sealant systems compared to traditional organotin catalysts such as dibutyltin dilaurate. Examples include one or more of bismuth neodecanoate, bismuth isooctanoate, and bismuth naphthenate. They are primarily used to provide basic curing catalytic activity for two-component silicone structural sealants at room temperature. Temperature-reversible phase change microcapsules are core-shell structures that can rupture and release their internal core material when the curing environment temperature is ≤5℃.
[0026] Melamine-formaldehyde resin and polyurethane composite wall material is a thermo-responsive phase change microcapsule wall material composed of an amino resin formed by the condensation polymerization of melamine and formaldehyde and a polyurethane resin formed by the polymerization of isocyanate and polyol. The core material of the thermo-responsive phase change microcapsules is an internal functional component completely encapsulated by the melamine-formaldehyde resin and polyurethane composite wall material, simultaneously serving as a temperature-responsive trigger carrier and a low-temperature catalytic active source. Tetradecane is a straight-chain alkane with a melting point of 5-6°C; it is liquid above its melting point and solid below it. The highly active titanium-based co-catalyst is a titanium-based complex with higher catalytic activity than low-activity organobismuth catalysts, capable of effectively catalyzing the condensation curing reaction of two-component silicone-structured sealants at low temperatures.
[0027] As can be seen from the above, the two-component silicone structural sealant provided in this application embodiment has component A based on α,ω-dihydroxypolydimethylsiloxane as the base polymer, combined with reinforcing fillers and composite silane coupling agents to construct the basic adhesive body. Component B uses a silane crosslinking agent to provide crosslinking reaction sites, combined with a low-activity organic bismuth catalyst to provide basic catalytic activity at >5°C. Simultaneously, a thermotropic phase change microcapsule of melamine-formaldehyde resin and polyurethane composite wall material is used to encapsulate n-tetradecane and a highly active titanium-based cocatalyst as the core material. At >5°C, the wall material of the thermotropic phase change microcapsule remains intact, effectively isolating and sealing the highly active titanium-based cocatalyst, preventing it from prematurely participating in the reaction and causing adverse reactions. The system's storage stability decreases. Under construction conditions of ≤5℃, the tetradecane phase change in the core material of the temperature-reactive phase change microcapsules causes rupture, releasing a highly active titanium-based co-catalyst. This highly active titanium-based co-catalyst and the low-activity organic bismuth catalyst form a low-temperature synergistic catalytic effect, accelerating the condensation and crosslinking reaction rate between the silane crosslinking agent and α,ω-dihydroxypolydimethylsiloxane. At the same time, it makes the crosslinking reaction more complete. Combined with the interfacial reinforcement effect of reinforcing fillers and composite silane coupling agents, it can effectively improve the problems of slow curing speed and low crosslinking density of existing two-component silicone structural sealants under low-temperature construction conditions of ≤5℃, which leads to permanent failure of bonding strength and elastic recovery rate.
[0028] In some embodiments, the composite silane coupling agent is a compound comprising an aminosilane coupling agent and an epoxysilane coupling agent.
[0029] It can be understood that aminosilane coupling agents are silane coupling agents containing amino functional groups in their molecules, such as one or more of γ-aminopropyltriethoxysilane, γ-aminopropyltrimethoxysilane, and N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane. Epoxysilane coupling agents are silane coupling agents containing epoxy functional groups in their molecules, such as one or more of γ-glycidoxypropyltrimethoxysilane and β-(3,4-epoxycyclohexyl)ethyltrimethoxysilane. The mass ratio of aminosilane coupling agent to epoxysilane coupling agent can be 1:1 to 3:1.
[0030] This configuration, through the combined use of aminosilane coupling agents and epoxysilane coupling agents, can simultaneously improve the adhesion performance of two-component silicone structural sealants to both inorganic substrates (such as glass, metal, and concrete) and organic substrates, improve the uniformity of the dispersion of reinforcing fillers in the base polymer, enhance interfacial bonding, and help improve the integrity of the crosslinking network. It can also form a relatively uniform three-dimensional structure when cured at ≤5℃, further improving the tensile strength and elastic recovery rate of the two-component silicone structural sealant.
[0031] In some embodiments, the particle size of the temperature-reactive phase change microcapsules is 5 μm to 10 μm, and the thickness of the wall material of the temperature-reactive phase change microcapsules is 0.5 μm to 1 μm.
[0032] It is understandable that the particle size is the average particle size of the thermo-responsive phase change microcapsules, which can be measured using a laser particle size analyzer and expressed as the volume average particle size D50. The wall thickness is the average thickness of the shell layer in the core-shell structure of the thermo-responsive phase change microcapsules, which can be obtained by observing and measuring the cross-section of the ruptured thermo-responsive phase change microcapsules using a scanning electron microscope (SEM).
[0033] This configuration, with a particle size range of 5μm to 10μm, ensures uniform dispersion of the thermo-responsive phase change microcapsules in the B-component base system, preventing agglomeration and sedimentation, while also maintaining the application flowability of the two-component silicone structural sealant. A wall thickness range of 0.5μm to 1μm balances the room-temperature stability and low-temperature rupture performance of the thermo-responsive phase change microcapsules. This ensures the microcapsules maintain structural integrity during preparation, room-temperature storage, and application through a static mixer, preventing premature release of the highly active titanium-based co-catalyst. Furthermore, in low-temperature application environments (≤5℃), the microcapsules achieve stable rupture through low-temperature embrittlement of the wall material combined with localized stress concentration caused by the phase change of the core material, allowing for timely release of the highly active titanium-based co-catalyst to participate in the curing reaction.
[0034] In some embodiments, the mass ratio of n-tetradecane to highly active titanium-based cocatalyst in the core material of the temperature-reversible phase change microcapsule is 93~97:3~7.
[0035] It can be understood that the mass ratio of n-tetradecane to the highly active titanium-based co-catalyst is the ratio of the mass of n-tetradecane to the mass of the highly active titanium-based co-catalyst.
[0036] This configuration, with a mass ratio of 93~97:3~7, ensures that n-tetradecane undergoes a stable liquid-solid phase transition at ≤5℃, generating sufficient local stress concentration to assist in wall material rupture. Simultaneously, it ensures the core material contains a sufficient amount of highly active titanium-based co-catalyst, which, upon release, forms an effective synergistic catalytic effect with the less active organic bismuth catalyst, significantly improving the curing speed and crosslinking density. If the proportion of highly active titanium-based co-catalyst is too high, it will affect the phase transition performance of n-tetradecane and may also lead to a decrease in the storage stability of the temperature-reversible phase transition microcapsules; if the proportion is too low, it will not provide sufficient low-temperature catalytic activity, making it difficult to achieve the desired curing effect.
[0037] In some embodiments, the highly active titanium-based cocatalyst is diisopropyl di(acetylacetonyl)titanate.
[0038] Diisopropyl di(acetylacetonate)titanate is a chelating titanate catalyst containing two acetylacetonate chelating groups and two isopropoxy groups in its molecule. It exhibits good chemical stability and is not prone to hydrolytic deactivation. Diisopropyl di(acetylacetonate)titanate demonstrates good dispersibility and compatibility in n-tetradecane, allowing for uniform dispersion within the core material. Its catalytic activity is higher than that of conventional organobismuth catalysts, maintaining high catalytic efficiency even at low temperatures (≤5℃). Furthermore, it exhibits no antagonistic effect with low-activity organobismuth catalysts; their synergistic use can significantly enhance the catalytic effect.
[0039] This setup, using diisopropyl di(acetylacetonate)titanate as a highly active titanium-based co-catalyst, can improve the long-term stability of the core material system, reduce catalyst deactivation during the temperature-reversible phase change microcapsule encapsulation process and room temperature storage, and its excellent low-temperature catalytic activity can effectively compensate for the insufficient activity of low-activity organic bismuth catalysts at low temperatures, accelerate the curing speed of two-component silicone structural sealant at ≤5℃, increase the final crosslinking density, and thus improve the bonding strength and elastic recovery rate of the sealant after low-temperature curing.
[0040] Please see Figure 1 The second aspect of this application provides a method for preparing a two-component silicone structural sealant, applied to a sealant preparation system. The sealant preparation system includes a stirring execution module and a temperature control module. The method includes: S100, α,ω-dihydroxy polydimethylsiloxane, reinforcing filler, and composite silane coupling agent are mixed evenly to obtain component A.
[0041] The sealant preparation system is understood to be equipment used to implement the preparation process of two-component silicone structural sealant. It primarily performs operations such as material mixing, stirring and dispersion, temperature control, process parameter monitoring, and closed-loop control of operating parameters. The sealant preparation system includes a reaction vessel, a stirring execution module, a temperature control module, and a control module. The reaction vessel is a sealed container for the mixing and dispersion process of the two-component silicone structural sealant. It includes a vessel body, a lid, an inlet, an outlet, and a sealing assembly. The lid is sealed and installed on the top of the vessel body, the inlet is located on the lid, and the outlet is located at the bottom of the vessel body. The sealing assembly ensures that the space inside the reaction vessel is isolated from the external environment, preventing moisture and oxygen from entering the reaction vessel and causing premature cross-linking and curing of the components of the two-component silicone structural sealant. It also prevents leakage of materials inside the reaction vessel during stirring.
[0042] The sealing assembly includes a static sealing assembly between the vessel body and the vessel lid, and a dynamic sealing assembly where the stirring shaft of the stirring execution module passes through the vessel lid. The static sealing assembly is located between the top end face of the vessel body and the bottom end face of the vessel lid, and includes a lower flange welded to the top of the vessel body, an upper flange welded to the bottom of the vessel lid, an annular sealing gasket sandwiched between the mating surfaces of the two flanges, and fastening bolts and lock nuts sequentially passing through corresponding bolt holes. By evenly tightening all the lock nuts, the upper and lower flanges are tightly fitted, compressing the annular sealing gasket to produce elastic deformation that fills the microscopic gaps between the flange mating surfaces, thus achieving a static seal between the fixed components.
[0043] The dynamic sealing assembly is located at the center opening on the top of the vessel lid. It includes a stationary ring fixed inside the center opening of the vessel lid, a rotating ring fixed on the stirring shaft of the stirring execution module and rotating synchronously with the shaft, a spring and spring seat sleeved on the stirring shaft, an auxiliary sealing ring, and a sealing cap fixed on the outside of the vessel lid. The two ends of the spring abut against the spring seat and the upper end face of the rotating ring, respectively, and always provide a downward elastic force to push the end faces of the rotating ring and the stationary ring to fit tightly to form a rotating sealing surface. The auxiliary sealing rings respectively realize the static seal between the rotating ring and the stirring shaft, and between the stationary ring and the vessel lid, thereby realizing the dynamic seal between the rotating stirring shaft and the fixed vessel lid.
[0044] The stirring execution module is an actuator for stirring and dispersing materials. It is installed on the lid of the reactor and includes a stirring drive motor, a stirring shaft, a stirring paddle, and a speed sensor. The stirring drive motor is fixedly mounted at the top center of the lid. The upper end of the stirring shaft is fixedly connected to the output shaft of the stirring drive motor, and the lower end extends vertically through the central opening of the lid into the material inside the reactor. The stirring paddle is fixedly mounted at the lower end of the stirring shaft and rotates synchronously with it. The speed sensor is installed on the output shaft of the stirring drive motor, coaxially with it. During operation, after the stirring drive motor is powered on, it drives the stirring shaft and stirring paddle to rotate synchronously, stirring and dispersing the materials inside the reactor. The speed sensor collects the speed signal of the stirring drive motor's output shaft in real time and transmits it to the control module.
[0045] The temperature control module is an actuator for precise temperature regulation of materials, comprising a heat exchange jacket, a circulating temperature control unit, and a temperature sensor. The heat exchange jacket is welded and fixed to the outer wall of the vessel, completely covering its side walls and bottom, forming a sealed medium flow chamber inside. The circulating temperature control unit is connected to the medium inlet and outlet of the heat exchange jacket via inlet and outlet pipes, respectively, forming a closed medium circulation loop. The temperature sensor extends through the vessel lid into the material inside the vessel, with the probe in direct contact with the material. During operation, the circulating temperature control unit outputs a cooling or heating medium at a set temperature according to instructions. The medium flows into the flow chamber of the heat exchange jacket through the inlet pipe, exchanges heat with the material inside the vessel, and then flows back to the circulating temperature control unit through the outlet pipe, thus regulating the material temperature. The temperature sensor collects the actual temperature signal of the material inside the vessel in real time and transmits it to the control module.
[0046] The stirring execution module and temperature control module are electrically connected to the control module. The control module receives real-time signals from the speed sensor and temperature sensor, compares the actual speed and temperature with preset control parameters, and sends speed adjustment commands to the stirring drive motor and power adjustment commands to the circulating temperature control unit based on the comparison results. This dynamically adjusts the stirring speed and temperature control output power, achieving dual-dimensional closed-loop control of the material dispersion process. This ensures that the inverse temperature response phase change microcapsules are not sheared and destroyed during dispersion, while simultaneously achieving uniform dispersion.
[0047] For example, α,ω-dihydroxy polydimethylsiloxane, reinforcing filler, and composite silane coupling agent are added to a reactor in the corresponding weight ratio. The mixture is stirred in stages using a stirring module. After the mixture is free of obvious particles, it is subjected to vacuum degassing to obtain a uniform, bubble-free component A. For instance, α,ω-dihydroxy polydimethylsiloxane is first added to a dry reactor. The stirring module is turned on, and the stirring speed is controlled within the range of 500 r / min to 1500 r / min. After stirring for 10 to 30 minutes, the reinforcing filler is added in 2 to 3 portions, with stirring for 15 to 20 minutes after each addition. Then, the composite silane coupling agent is added, and stirring continues for 30 to 60 minutes. Finally, degassing is performed under a vacuum of -0.08 MPa to -0.1 MPa for 10 to 20 minutes to obtain component A.
[0048] S200, the silane crosslinking agent and the low-activity organic bismuth catalyst are mixed evenly to obtain the basic system of component B.
[0049] It is understandable that the basic system of component B is a basic catalytic crosslinking system formed by premixing silane crosslinking agent and low-activity organic bismuth catalyst. It is the core component of component B. No temperature-reactive phase change microcapsules are added. It mainly provides basic crosslinking reaction sites and catalytic activity at room temperature.
[0050] For example, silane crosslinking agent and low-activity organobismuth catalyst are added to a dry, sealed reactor in corresponding weight ratios. The mixture is then stirred at low speed using a stirring module, ensuring complete isolation from air moisture to obtain a transparent and homogeneous component B base system. Alternatively, silane crosslinking agent is added to a pre-dried and dehydrated reactor, the reactor lid is closed and sealed, the stirring module is activated, and the stirring speed is controlled within the range of 300 r / min to 800 r / min. After stirring for 5 to 10 minutes, the low-activity organobismuth catalyst is slowly added, and stirring continues for 20 to 40 minutes, maintaining a relative humidity below 30% within the reactor throughout the process to obtain the component B base system.
[0051] S300 is obtained by uniformly mixing n-tetradecane with a highly active titanium-based co-catalyst to obtain the core material of temperature-reversible phase change microcapsules.
[0052] For example, tetradecane and a highly active titanium-based co-catalyst are added to a dry, sealed reactor at a preset mass ratio. The mixture is then stirred at low speed using a stirring module until a homogeneous and stable solution is formed, thus obtaining the core material for the temperature-reversible phase change microcapsules. Alternatively, tetradecane can be added to a pre-dried and dehydrated reactor, the reactor lid closed and sealed, the stirring module activated, and the stirring speed controlled within the range of 200 r / min to 500 r / min. After stirring for 5 to 10 minutes, a highly active titanium-based co-catalyst is added at a mass ratio of 93–97:3–7, and stirring continues for 30 to 60 minutes until no significant stratification occurs, thus obtaining the core material.
[0053] S400 uses melamine-formaldehyde resin and polyurethane composite wall material to coat and cure the core material, resulting in temperature-reversible phase change microcapsules.
[0054] It is understandable that coating and curing is a process in which functionalized wall material layers are sequentially formed on the surface of the core material through a stepwise polymerization process, and the wall material is cured and molded through a cross-linking reaction, completely sealing and encapsulating the core material inside.
[0055] For example, a process combining stepwise interfacial polymerization and in-situ polymerization is adopted. First, a polyurethane isolation layer is formed on the surface of the core material, and then a rigid outer layer of melamine-formaldehyde resin is formed outside the isolation layer. After curing, filtration, washing and drying, inverse temperature responsive phase change microcapsules are obtained. For example, the core material and emulsifier are first added to deionized water, and the stirring speed is controlled by the stirring execution module to emulsify at high speed within the range of 8000 r / min to 12000 r / min for 15 to 30 minutes to form a stable oil-in-water emulsion. Then, isocyanate monomers and polyol monomers are added to the oil-in-water emulsion, and the reaction is carried out at 40°C to 60°C for 1 to 2 hours to form a polyurethane isolation layer. Next, melamine-formaldehyde prepolymer is added, the pH value is adjusted to 4 to 5 with dilute hydrochloric acid, and the temperature is raised to 70°C to 80°C to react for 2 to 3 hours to form a melamine-formaldehyde resin outer layer. After the reaction is completed, the product is collected by filtration, washed 3 to 5 times with deionized water, and vacuum dried at 50°C to 60°C for 12 to 24 hours to obtain inverse temperature response phase change microcapsules.
[0056] S500 adds temperature-reactive phase change microcapsules to the B-component base system, stirs and disperses them, and obtains shear stress and temperature information of the B-component base system. The shear stress information is used to reflect the magnitude of the shear impact on the temperature-reactive phase change microcapsules during the dispersion process, and the temperature information is used to reflect the temperature fluctuation of the B-component base system during the dispersion process.
[0057] Shear stress information is understood to be a physical quantity reflecting the magnitude of the shear force per unit area within a fluid. It is used to quantitatively characterize the shear impact intensity exerted by material flow on the wall material of the temperature-inverse response phase change microcapsules during stirring and dispersion, and can be acquired through an online rheometer. Temperature information is a physical quantity reflecting the overall temperature level and real-time changes of the B-component base system, and is acquired through a temperature sensor in direct contact with the material.
[0058] For example, the temperature-reactive phase change microcapsules are slowly added to a reactor containing the B-component base system according to the corresponding weight ratio. The mixture is dispersed by low-speed stirring using a stirring module, while shear stress information is collected by an online rheometer and temperature information is collected by a temperature sensor in the temperature control module. All collected information is transmitted to the control module in real time. For instance, during stirring, the temperature-reactive phase change microcapsules are slowly added to the reactor in 3 to 5 portions, with stirring for 10 to 15 minutes after each addition, controlling the stirring speed within the range of 200 to 600 r / min. During dispersion, shear stress information is collected in real time by an online rheometer installed on the side wall of the reactor at a frequency of 1 to 3 times per second, and temperature information is collected in real time by a temperature sensor inserted 10 to 15 cm below the liquid surface, at the same frequency as the shear stress information. All collected information is transmitted to the control module for storage and subsequent processing.
[0059] The S600 controls the rotation speed of the stirring execution module based on shear stress information and controls the output power of the temperature control module based on temperature information to obtain a uniformly dispersed component B.
[0060] It can be understood that rotational speed is the number of revolutions per minute (r / min) of the stirring shaft of the stirring execution module. Output power is the cooling or heating energy output per unit time of the circulating temperature control unit of the temperature control module, in kW. Uniform dispersion means that the inverse temperature response phase change microcapsules show no obvious agglomeration or sedimentation in the B-component base system, and are uniformly distributed in the B-component base system.
[0061] Please see Figure 2 In some embodiments, S600, controlling the rotational speed of the stirring execution module based on shear stress information includes: S610, based on the wall material structure characteristics of the temperature-reactive phase change microcapsules, determines the upper limit threshold of the non-rupture shear stress of the temperature-reactive phase change microcapsules.
[0062] It is understandable that the structural characteristics of the wall material refer to the physical structural properties of the composite wall material of the temperature-reactive phase change microcapsules, including the material composition, wall thickness, hardness, elastic modulus, and tensile strength. The upper limit threshold of the non-rupture shear stress is the maximum shear stress value that the wall material of the temperature-reactive phase change microcapsules can withstand. When the actual shear stress exceeds this threshold, the wall material of the temperature-reactive phase change microcapsules will rupture, causing the internal core material to be released prematurely.
[0063] For example, the prepared thermo-responsive phase change microcapsules are first dispersed in inert silicone oil with a viscosity of 500~2000 mPa·s to prepare a suspension with a mass concentration of 0.05%~0.2%. After ultrasonic dispersion for 3~10 min to ensure that the thermo-responsive phase change microcapsules do not agglomerate, a universal material testing machine equipped with a cylindrical flat-head indenter is used to conduct single-particle compression tests on 15~30 thermo-responsive phase change microcapsules within the target particle size range at a loading rate of 0.2~1 mm / min. At the same time, the rupture of the thermo-responsive phase change microcapsules is observed in real time using an optical microscope, and the loading force at the rupture of each thermo-responsive phase change microcapsule is recorded. Then, the shear stress at the rupture of each thermo-responsive phase change microcapsule is calculated using the shear stress calculation formula, and the rupture rate of the thermo-responsive phase change microcapsules under different shear stresses is statistically analyzed. The maximum shear stress corresponding to a rupture rate of less than 1% is used as the upper limit threshold of the non-rupture shear stress.
[0064] For example, a suspension with a mass concentration of 0.1% was prepared using dimethyl silicone oil with a viscosity of 1000 mPa·s, ultrasonically dispersed for 5 min, and tested using a flat-head indenter with a diameter of 1 mm at a loading rate of 0.5 mm / min for 20 temperature-sensitive phase change microcapsules with particle sizes ranging from 5 μm to 10 μm. The upper limit threshold of the non-rupture shear stress for the temperature-sensitive phase change microcapsules (wall thickness 0.5 μm to 1 μm) of melamine-formaldehyde resin and polyurethane composite wall material obtained by the above method is usually 50 Pa to 100 Pa.
[0065] S611, based on the rheological properties of the B-component basic system, determines the lower threshold of effective dispersion shear stress for inverse temperature response phase change microcapsules.
[0066] Rheological properties are understood to be the flow and deformation characteristics of a fluid under external forces, including viscosity, shear rate, shear stress, and thixotropy. The effective dispersion shear stress lower limit threshold is the minimum shear stress value required for the inverse-temperature response phase change microcapsules to achieve uniform dispersion in a component B-based system without agglomeration or sedimentation.
[0067] For example, a rotational rheometer equipped with a parallel plate rotor was used to test the B-component basic system under isothermal conditions of 20~30℃ for 1 second. -1 up to 1000s -1 Steady-state rheological tests were conducted within a range, recording the shear stress values corresponding to different shear rates. Samples were taken after holding the shear at each shear rate for 3–10 minutes, and the particle size distribution of the thermotropic response phase change microcapsules was measured using a laser particle size analyzer. The minimum shear stress corresponding to a particle size distribution D90 ≤ 15 μm and a settling layer height not exceeding 5% of the total height after 24 hours of settling was used as the lower limit threshold for effective dispersion shear stress. For example, using a 40 mm diameter parallel plate rotor with a 1 mm plate spacing, tests were conducted at a constant temperature of 25 °C, holding the shear at each shear rate for 5 minutes. For a component B-based system with a viscosity ranging from 1000 mPa·s to 5000 mPa·s, the lower limit threshold for effective dispersion shear stress obtained from the tests was typically 10 Pa to 30 Pa.
[0068] S612, based on the upper limit threshold of the non-ruptured shear stress and the lower limit threshold of the effective dispersed shear stress, the safe operating range of shear stress for the temperature-reversible phase change microcapsule is obtained.
[0069] It can be understood that the safe working range of shear stress is the range of shear stress values that simultaneously meet the requirements of preventing the microcapsules from rupturing and effectively dispersing them in response to temperature inversion phase change. Its lower limit is the lower threshold of effective dispersion shear stress, and its upper limit is the upper threshold of non-rupture shear stress.
[0070] For example, the effective dispersed shear stress lower limit threshold obtained from the test is used as the lower limit of the interval, and the non-rupture shear stress upper limit threshold is used as the upper limit of the interval. The numerical range between the two is the safe working range of shear stress.
[0071] S613, the measured value of shear stress is obtained based on shear stress information.
[0072] It can be understood that the measured value of shear stress is a numerical value that accurately reflects the actual shear stress of the material during the dispersion process, obtained by analyzing and processing the collected shear stress information. The unit is Pascal (Pa).
[0073] Please see Figure 3 In one possible implementation, S613, the measured value of shear stress is obtained based on the shear stress information, including: S6131, based on shear stress information, obtains the associated parameters of fluid shear action.
[0074] It is understandable that fluid shearing parameters are raw physical quantities directly related to the internal shearing action of the fluid, collected by an online rheometer, including torque, rotational speed, and shear rate.
[0075] For example, an online rheometer installed on the side wall of the reactor measures the torque and rotational speed of the rotor as it rotates in the fluid to obtain the corresponding fluid shear parameters, and transmits these fluid shear parameters to the control module in real time.
[0076] S6132, based on the rheological properties of the B-component basic system and the actual operating status of the stirring execution module, constructs a parameter conversion correspondence.
[0077] It is understandable that the parameter conversion correspondence is the mathematical mapping relationship between the fluid shearing action-related parameters and the actual shear stress.
[0078] For example, steady-state rheological tests are performed on the B-component base system using a rotational rheometer to collect shear stress data at different shear rates. The collected shear stress data is then substituted into common fluid rheological models for fitting. The model with the closest correlation coefficient to 1 is used as the rheological model for the B-component base system, and the corresponding rheological parameters are obtained. Combined with the geometric parameters of the stirring impeller of the stirring execution module, the correspondence between stirring speed and shear rate is obtained through fluid dynamics calculations. Finally, a linear or nonlinear conversion formula is established between fluid shear action parameters such as torque and speed and the actual shear stress, which is the parameter conversion correspondence.
[0079] For example, the B-component basic system was tested using a cone-plate rotational rheometer under isothermal conditions of 25°C, with the shear rate range set to 1 s. -1up to 1000s -1 Every 10 seconds -1 A set of data on the relationship between shear rate and shear stress was collected; the collected 20 sets of experimental data were then substituted into the Newtonian fluid model (τ=μ×γ) and the pseudoplastic fluid model (τ=K×γ). n ) and Bingham fluid model (τ=τ0+μ p The least squares method was used to fit the model using ×γ), and the correlation coefficient R² = 0.998 was found to be closest to 1 for the pseudoplastic fluid model. Therefore, the basic system of component B was determined to be a pseudoplastic fluid, with the corresponding rheological parameter being the consistency coefficient K = 12.5 Pa·s. n The mobility behavior index n=0.72.
[0080] The device constant k = 1.2s⁻¹ / (r / min) of the stirring execution module was obtained through experimental calibration, that is, the shear rate γ = 1.2×N (N is the stirring speed, in r / min).
[0081] Based on the calibration relationship between torque and shear stress of the rotating rheometer, T=K0×τ (where K0 is the rheometer rotor constant, K0=0.0002N·m / Pa in this embodiment), the complete parameter conversion formula is finally derived: τ=T / 0.0002, and τ=12.5×(1.2×N). 0 · 7 ², meaning that shear stress can be calculated directly from torque or indirectly from stirring speed.
[0082] S6133, based on the parameter conversion correspondence, the fluid shear action related parameters are subjected to directional analytical transformation to obtain the transformed fluid shear action related parameters.
[0083] It can be understood that directional analytical transformation is the process of substituting the collected original fluid shear parameters into a pre-built parameter conversion correspondence to calculate intermediate parameters directly related to the actual shear stress. These intermediate parameters are transitional values generated during the calculation process and used to derive the final result.
[0084] For example, the torque and speed values collected by the online rheometer are substituted into the parameter conversion formula established in S6132 to calculate the corresponding intermediate shear stress value, which is the fluid shear action correlation parameter after conversion.
[0085] S6134, after the transformation, the associated parameters of fluid shearing are uniformly normalized to obtain the measured value of shear stress.
[0086] It is understandable that uniform normalization involves filtering, averaging, and outlier removal of the parameters related to fluid shear after conversion, thereby reducing the impact of measurement noise and random errors.
[0087] For example, the moving average method combined with the 3σ criterion is used for data processing. A sliding window is taken as a continuous 5 to 20 fluid shear action correlation parameters after conversion. The average value and standard deviation of the data within the sliding window are calculated. After removing outliers that deviate from the average value by more than 3 times the standard deviation, the average value of the remaining valid data is calculated again as the measured value of shear stress at the current moment. The sliding window is updated every 0.5 to 2 seconds to achieve real-time output of the measured value of shear stress.
[0088] By employing the steps S6131 to S6134 described above, the raw signals acquired by the online rheometer can be accurately converted into measured values of shear stress that reflect the actual shear action, effectively reducing measurement errors and noise interference, and improving the accuracy and reliability of shear stress control.
[0089] S614. The measured value of shear stress is compared with the safe working range of shear stress to obtain the comparison result.
[0090] It is understandable that the comparison result is the positional relationship between the measured shear stress value and the safe working range of shear stress.
[0091] For example, the control module compares the measured value of shear stress obtained in real time with the upper limit threshold of the non-rupture shear stress and the lower limit threshold of the effective dispersed shear stress in the safe range of shear stress, and generates the corresponding comparison results.
[0092] S615 controls the rotation speed of the stirring execution module based on the comparison results.
[0093] For example, when the comparison result shows that the measured shear stress is within the safe range of shear stress, the current stirring speed is kept unchanged; when the comparison result shows that the upper limit threshold of the non-rupture shear stress is higher than the safe range of shear stress, the stirring speed is reduced by a preset step size until the shear stress returns to the safe range of shear stress; when the comparison result shows that the lower limit threshold of the effective dispersion shear stress is lower than the safe range of shear stress, the stirring speed is increased by a preset step size until the effective dispersion effect is achieved.
[0094] By adopting the above steps S610 to S615, adaptive closed-loop control of stirring speed can be achieved, so that the shear stress during the dispersion process is always kept within the safe working range of shear stress. This effectively reduces the premature rupture of the inverse temperature response phase change microcapsules caused by excessive shear stress, and ensures that the shear stress is sufficient to achieve uniform dispersion of the inverse temperature response phase change microcapsules, significantly improving the stability and reliability of the B component preparation process.
[0095] Please see Figure 4 In some embodiments, S600, controlling the output power of the temperature control module based on temperature information includes: S620, based on temperature information, obtains the correlation parameters of the overall thermal environment of the B-component basic system.
[0096] It is understandable that correlation parameters are physical quantities that can reflect the temperature state and changing trend of the basic system of component B, including real-time temperature, temperature change rate, temperature distribution uniformity, etc.
[0097] For example, temperature information is collected by multiple temperature sensors evenly distributed in different positions inside the reactor. The control module calculates the real-time average temperature by averaging the collected values from multiple temperature sensors. The temperature change rate is obtained by calculating the ratio of the temperature difference between two adjacent collection times to the time interval. The temperature distribution uniformity is obtained by calculating the standard deviation of the temperature at different positions. These parameters together constitute the correlation parameters of the overall thermal environment.
[0098] S621, based on the associated parameters, the continuous heat load properties of the B-component basic system, and the temperature tolerance characteristics of the inverse-temperature response phase change microcapsules, establishes the power regulation benchmark for the temperature control module.
[0099] It is understandable that the continuous heat load attribute refers to heat transfer-related properties of the B-component base system, such as mass, specific heat capacity, and stirring heat generation rate. The power adjustment reference is the correspondence between the output power of the temperature control module and the temperature of the B-component base system, used to guide the control module to adjust the temperature control power according to temperature changes.
[0100] Please see Figure 5 In one possible implementation, S621, based on the associated parameters, the continuous heat load properties of the B-component base system, and the temperature tolerance characteristics of the inversion-response phase change microcapsules, a power regulation reference for the temperature control module is established, including: S6211, based on the temperature tolerance characteristics of inverse temperature response phase change microcapsules, determines the temperature constraint range suitable for the B-component base system.
[0101] It can be understood that temperature tolerance characteristics refer to the temperature range within which the inverse-temperature-responsive phase change microcapsules can maintain their structural integrity and prevent premature rupture. Temperature constraint range refers to the temperature range of the B-component base system that ensures the structural integrity of the inverse-temperature-responsive phase change microcapsules and prevents premature rupture.
[0102] For example, the temperature tolerance of the inverse-temperature response phase change microcapsules was tested using a high and low temperature test chamber. The rupture of the inverse-temperature response phase change microcapsules at different temperatures was observed, and the temperature range corresponding to a rupture rate of less than 1% was taken as the temperature constraint range.
[0103] S6212, Based on the continuous heat load properties of the B-component basic system, generate the corresponding heat load constraint conditions for the B-component basic system.
[0104] It is understandable that the heat load constraint is a limitation imposed on parameters such as the maximum output power and medium flow rate of the circulating temperature control unit in order to ensure that the temperature control module can effectively regulate the temperature of the B-component base system.
[0105] For example, based on the total mass and specific heat capacity of the B-component basic system in the reactor, as well as the stirring heat generation rate during the stirring process, and combined with the maximum temperature change rate required by the process, the maximum cooling power and maximum heating power required by the temperature control module are calculated using the heat balance principle, and these are used as heat load constraints. The heat balance principle states that the algebraic sum of the power output by the temperature control module and the stirring heat generation power equals the heat power required for the temperature change of the B-component basic system.
[0106] For example, for a 1000L B-component base system, with a total mass of 950kg, a specific heat capacity of 1800J / (kg·℃), and a stirring heat generation rate of 5kW (i.e., the heat continuously input into the system during stirring), and a maximum temperature change rate of 1℃ per minute as required by the process, first calculate the heat power required for a 1℃ temperature change in the B-component base system. Multiply the total mass by the specific heat capacity and then by 1℃ per minute to convert it to a temperature change per second, resulting in 28500W, or 28.5kW. Then calculate the maximum cooling power requirement. When the B-component base system needs to be cooled, the cooling power must simultaneously offset the stirring... The heat required for heat generation and system cooling is calculated. Therefore, the heat power required for temperature change of the B-component base system plus the stirring heat generation rate is 33.5kW. Taking a safety factor of 1.2, the maximum cooling power requirement is finally determined to be 40kW. Next, the maximum heating power requirement is calculated. When the B-component base system needs to be heated, the stirring heat generation can assist in heating. Therefore, the heat power required for temperature change of the B-component base system minus the stirring heat generation rate is 23.5kW. Again, taking a safety factor of 1.2, the maximum heating power requirement is finally determined to be 28kW. This is used as the heat load constraint condition under this production scale.
[0107] S6213, based on the associated parameters, performs a unified adaptation and correction on the temperature constraint range and the heat load constraint conditions to obtain the corrected composite constraint conditions.
[0108] It is understandable that unified adaptation correction involves dynamically adjusting the temperature constraint range and heat load constraint conditions based on the actual thermal environment of the B-component base system, so that the two are matched and the temperature control system can operate stably.
[0109] For example, when the temperature distribution uniformity of the B component base system is poor, the difference between the upper and lower limits of the temperature constraint range is appropriately reduced, while the power adjustment accuracy of the temperature control module is improved; when the system heat load is large, the upper limit of the power of the heat load constraint condition is appropriately increased to ensure that the temperature control requirements can be met.
[0110] S6214 integrates and corrects the composite constraint conditions to obtain the power regulation reference of the temperature control module.
[0111] For example, the corrected temperature constraint range is divided into multiple sub-intervals, and a corresponding power adjustment coefficient is set for each sub-interval. Simultaneously, the maximum allowable power for each sub-interval is set in conjunction with the heat load constraint conditions, and the combined results yield a complete power adjustment benchmark. For instance, the temperature range of 10℃ to 30℃ is divided into three sub-intervals: 10℃ to 15℃, 15℃ to 25℃, and 25℃ to 30℃, with corresponding power adjustment coefficients of 0.8, 0.5, and 1.0, respectively. The maximum allowable power for each sub-interval is 15kW, 10kW, and 20kW, respectively.
[0112] By adopting the above steps S6211 to S6214, a reasonable temperature control power adjustment benchmark can be established, fully considering the temperature tolerance characteristics of the inverse temperature response phase change microcapsules and the thermal load characteristics of the B component basic system, making the temperature control adjustment more precise and efficient, effectively reducing the premature rupture of the inverse temperature response phase change microcapsules caused by temperature anomalies, and ensuring the stable operation of the temperature control system.
[0113] S622 determines the power regulation requirements suitable for the current distributed operating conditions based on the dynamic change trend of the associated parameters and the power regulation benchmark.
[0114] It is understandable that the power regulation requirement is to keep the temperature of the B-component base system within a preset range, and the temperature control module needs to perform power adjustment in terms of direction and magnitude.
[0115] For example, the control module uses a preset target temperature and allowable temperature deviation as a benchmark, combined with the real-time temperature and temperature change rate of the B-component base system collected, to determine the power adjustment requirements. The target temperature is set to 18~22℃, the allowable temperature deviation to be ±0.5~±1.5℃, and the temperature change rate threshold to be ±0.1~±0.3℃ / min. When the real-time temperature is within the allowable temperature deviation range and the absolute value of the temperature change rate does not exceed the temperature change rate threshold, the current power is maintained. When the real-time temperature is higher than the upper limit of the allowable temperature range, or the temperature is within the allowable temperature range but the temperature change rate is greater than the positive temperature change rate threshold, the cooling power needs to be increased. When the real-time temperature is lower than the lower limit of the allowable temperature range, or the temperature is within the allowable temperature range but the temperature change rate is less than the negative temperature change rate threshold, the heating power needs to be increased. The power adjustment range is calculated using a proportional-integral control algorithm, with the formula ΔP=K. p ×ΔT+K i ×∫ΔTdt, where ΔP is the power adjustment of the temperature control module, in kW and K. p This is a proportionality coefficient, with a value ranging from 1 to 5 kW / ℃, K. iThe integral coefficient is 0.2~1kW / (℃·min), ΔT is the deviation between the real-time temperature and the target temperature in ℃, and ∫ΔTdt is the integral value of the temperature deviation over one control cycle in ℃·min. The proportional coefficient and integral coefficient can be adaptively adjusted according to the reactor volume and the system heat load.
[0116] S623 controls the output power of the temperature control module based on power regulation requirements.
[0117] For example, when it is determined that the cooling power needs to be increased, the control module sends a command to increase the compressor power and medium flow of the circulating temperature control unit; when it is determined that the heating power needs to be increased, a command is sent to increase the output power of the heating element; when it is determined that the power should remain unchanged, the current operating parameters are maintained.
[0118] By employing the above steps S620 to S623, precise closed-loop control of the temperature of the B-component base system can be achieved, ensuring that the temperature of the B-component base system is always kept within the tolerance range of the inverse temperature response phase change microcapsules. This effectively reduces the premature rupture of the inverse temperature response phase change microcapsules caused by excessively high or low temperatures, and ensures the isolation and sealing effect of the highly active titanium-based co-catalyst during preparation and storage.
[0119] S700, by sealing and storing components A and B separately, yields a two-component silicone structural sealant.
[0120] It is understandable that independent sealed storage involves placing the prepared components A and B into separate sealed containers to isolate them from air and moisture, thus preventing premature cross-linking and curing reactions.
[0121] For example, the prepared components A and B are respectively placed into sealed plastic or metal drums with anti-corrosion coating on the inner wall, dry nitrogen is introduced into the drums to remove air, and then the drums are sealed and stored in a cool and dry environment.
[0122] By adopting the above steps S100 to S700, a two-component silicone structural sealant with both excellent abnormal temperature storage stability and low temperature curing performance can be prepared. This effectively improves the problem in the prior art that the two-component silicone structural sealant has a slow curing speed and low crosslinking density in a low temperature construction environment of ≤5℃, which leads to the permanent failure of the bonding strength and elastic recovery rate to meet the standards.
[0123] The following description is based on specific embodiments.
[0124] Example 1 1) Prepare the raw materials for component A: 1000g of α,ω-dihydroxypolydimethylsiloxane (viscosity 20000mPa·s), 150g of stearic acid surface-modified nano-active calcium carbonate (particle size 80nm), 10g of γ-aminopropyltriethoxysilane (KH550), and 5g of γ-glycidyl etheroxypropyltrimethoxysilane (KH560).
[0125] 2) Prepare the raw materials for component B: 600g of methyltriethoxysilane, 20g of bismuth neodecanoate, and 150g of thermo-responsive phase change microcapsules; wherein the thermo-responsive phase change microcapsules are melamine-formaldehyde resin and polyurethane composite wall material with a particle size of 7μm and a wall thickness of 0.7μm, and the core material is a mixture of n-tetradecane and diisopropyl di(acetylacetonate)titanate in a mass ratio of 95:5.
[0126] 3) Preparation of component A: Add α,ω-dihydroxypolydimethylsiloxane to a dry jacketed stainless steel stirred reactor, turn on the stirring module, and stir at 800 r / min for 20 min; add surface-modified nano-activated calcium carbonate in two batches, stirring for 15 min after each addition; add composite silane coupling agent and continue stirring for 40 min; finally, degas under a vacuum of -0.09 MPa for 15 min to obtain component A.
[0127] 4) Preparation of the basic system of component B: Add methyltriethoxysilane to a pre-dried and dehydrated reaction vessel, close the vessel lid seal, turn on the stirring module, and stir at a speed of 500 r / min for 8 min; slowly add bismuth neodecanoate and continue stirring for 30 min, keeping the relative humidity inside the reaction vessel below 25% throughout the process to obtain the basic system of component B.
[0128] 5) Preparation of temperature-reactive phase change microcapsules: Tetradecane and diisopropyl di(acetylacetonyl)titanate were added to a dry and sealed reactor in a mass ratio, and stirred at 300 r / min for 40 min to obtain the core material. A combination of stepwise interfacial polymerization and in-situ polymerization was used to form a polyurethane isolation layer and a melamine-formaldehyde resin outer layer on the surface of the core material. After curing, filtration, washing and drying, temperature-reactive phase change microcapsules were obtained.
[0129] 6) Preparation of component B: The temperature-reversible phase change microcapsules were slowly added to the component B base system in 4 portions, with the stirring speed controlled at 400 r / min and stirring for 12 min after each addition. During the dispersion process, shear stress information was collected by an online rheometer and temperature information was collected by a temperature sensor. The control module dynamically adjusted the stirring speed and temperature control power to keep the shear stress at 30~70 Pa and the temperature at 18~22℃, so as to obtain a uniformly dispersed component B.
[0130] 7) Place component A and component B into sealed metal containers with an anti-corrosion coating on the inner wall, fill with dry nitrogen, and seal to obtain a two-component silicone structural sealant.
[0131] Example 2 1) Prepare the raw materials for component A: 900g of α,ω-dihydroxypolydimethylsiloxane (viscosity 30000mPa·s), 200g of stearic acid surface-modified nano-active calcium carbonate (particle size 60nm), 12g of γ-aminopropyltriethoxysilane (KH550), and 6g of γ-glycidyl etheroxypropyltrimethoxysilane (KH560).
[0132] 2) Prepare the raw materials for component B: 550g of methyltrimethoxysilane, 30g of bismuth isooctanoate, and 200g of thermo-responsive phase change microcapsules; wherein the thermo-responsive phase change microcapsules are melamine-formaldehyde resin and polyurethane composite wall material with a particle size of 5μm and a wall thickness of 0.5μm, and the core material is a mixture of n-tetradecane and di(acetylacetonyl)titanate in a mass ratio of 93:7.
[0133] 3) The preparation steps are the same as in Example 1.
[0134] Example 3 1) Prepare the raw materials for component A: 1100g of α,ω-dihydroxypolydimethylsiloxane (viscosity 15000mPa·s), 100g of fumed silica (specific surface area 200m² / g), 8g of γ-aminopropyltriethoxysilane (KH550), and 4g of γ-glycidyl etheroxypropyltrimethoxysilane (KH560).
[0135] 2) Prepare the raw materials for component B: 650g of vinyltrimethoxysilane, 10g of bismuth naphthenate, and 100g of thermo-responsive phase change microcapsules; wherein the thermo-responsive phase change microcapsules are melamine-formaldehyde resin and polyurethane composite wall material with a particle size of 10μm and a wall thickness of 1μm, and the core material is a mixture of n-tetradecane and di(acetylacetonyl)titanate in a mass ratio of 97:3.
[0136] 3) The preparation steps are the same as in Example 1.
[0137] Comparative Example 1 1) Prepare the raw materials for component A in exactly the same way as in Example 1.
[0138] 2) Prepare the raw materials for component B: 600g of methyltriethoxysilane and 20g of bismuth neodecanoate, without adding temperature-reversible phase change microcapsules.
[0139] 3) The preparation steps are the same as in Example 1, except that the preparation and addition steps of the temperature-reversible phase change microcapsules are omitted.
[0140] Comparative Example 2 1) Prepare the raw materials for component A in exactly the same way as in Example 1.
[0141] 2) Prepare the raw materials for component B: 600g of methyltriethoxysilane, 20g of bismuth neodecanoate, and 7.5g of diisopropyl di(acetylacetonyl)titanate. Add the titanium-based co-catalyst directly to the basic system of component B without microencapsulation.
[0142] 3) The preparation steps are the same as in Example 1, except that the preparation steps of the temperature-reversible phase change microcapsules are omitted, and the titanium-based co-catalyst and bismuth neodecanoate are added to the basic system of component B at the same time.
[0143] Comparative Example 3 1) Prepare the raw materials for component A in exactly the same way as in Example 1.
[0144] 2) Prepare the raw materials for component B: 600g of methyltriethoxysilane, 20g of bismuth neodecanoate, and 150g of single melamine-formaldehyde resin wall material microcapsules; wherein the core material of the microcapsules is the same as that in Example 1, except that the wall material is single melamine-formaldehyde resin with a particle size of 7μm and a wall thickness of 0.7μm.
[0145] 3) The preparation steps are the same as in Example 1.
[0146] Comparative Example 4 1) Prepare the raw materials for component A in exactly the same way as in Example 1.
[0147] 2) Prepare raw materials for component B: 600g of methyltriethoxysilane and 5g of dibutyltin dilaurate, using a traditional organotin catalyst system.
[0148] 3) The preparation steps are the same as in Example 1, except that the low-activity organic bismuth catalyst is replaced with dibutyltin dilaurate.
[0149] 1. The performance of the two-component silicone structural sealants prepared in all the above embodiments and comparative examples was tested using the following methods: Stability at room temperature: The sealed component B was placed in a 50℃ constant temperature chamber for accelerated thermal aging for 7 days. After removal, it was observed whether gelation, curing or obvious thickening occurred. At the same time, the change rate of surface drying time at 50℃ was tested.
[0150] Low-temperature curing speed: Under constant temperature and humidity conditions of 5℃ and 50% relative humidity, the surface drying time and complete curing time are tested according to GB / T13477.5-2002.
[0151] Tensile bond strength: The tensile bond strength was tested according to GB16776-2005 standard, after curing at 25℃ for 7 days and after curing at 5℃ for 14 days.
[0152] Elastic recovery rate: The elastic recovery rate was tested according to GB16776-2005 standard after 14 days of low-temperature curing at 5℃.
[0153] All performance tests are expressed as the mean ± standard deviation of three parallel experiments. The test results are shown in Table 1 below: Table 1 As shown in Table 1, Examples 1-3 employ a binary catalytic system using a low-activity organic bismuth catalyst and a thermo-responsive phase change microcapsule encapsulating a highly active titanium-based co-catalyst. Simultaneously, the thermo-responsive phase change microcapsules are non-destructively dispersed through a dual closed-loop control of shear stress and temperature. This maintains excellent room-temperature storage stability (the surface drying time change rate after 7 days of 50℃ heat aging is less than 10%) and significantly improves low-temperature curing performance (the complete curing time at 5℃ is shortened to 42-52 hours). Furthermore, the tensile bond strength and elastic recovery rate after low-temperature curing meet the requirements of GB16776-2005 standard.
[0154] Comparative Example 1 did not add temperature-reversible phase change microcapsules and only used a low-activity organic bismuth catalyst. Although the storage stability was good, the low-temperature curing speed was extremely slow, with a complete curing time of up to 168 hours at 5°C, and the mechanical properties after low-temperature curing were severely insufficient. Comparative Example 2 directly added a highly active titanium-based co-catalyst, which caused component B to completely gel and solidify during the 50°C thermal aging process, resulting in a complete loss of storage stability. Comparative Example 3 used a single melamine-formaldehyde resin wall material microcapsule, which had insufficient low-temperature embrittlement performance. Some microcapsules ruptured prematurely during storage, leading to decreased storage stability and poor low-temperature catalytic effect. Comparative Example 4 used a traditional organotin catalyst. Although the low-temperature curing performance was improved, the storage stability was poor, and there were environmental risks.
[0155] 2. Low-temperature rupture performance test of temperature-reversible phase change microcapsules: The temperature-reactive phase change microcapsules prepared in Examples 1-3 and the single melamine-formaldehyde resin wall material microcapsules prepared in Comparative Example 3 were subjected to low-temperature rupture performance tests, and the test methods are as follows: 2.1 Constant Temperature Static Bursting Rate Test Equal amounts of microcapsules were placed in constant temperature and humidity chambers at 5℃ and 25℃ and left to stand for 24 hours. Then, samples were dropped onto glass slides and observed using an optical microscope (magnification 1000×). The proportion of ruptured microcapsules in each field of view was counted. Ten fields of view were counted under each temperature condition, and the average value was taken.
[0156] The test results show that: The temperature-reversible phase change microcapsules of Example 1 had a rupture rate of 92.3% at 5°C and 0.7% at 25°C.
[0157] The temperature-reversible phase change microcapsules of Example 2 had a rupture rate of 94.1% at 5°C and 0.5% at 25°C.
[0158] The temperature-reversible phase change microcapsules of Example 3 had a rupture rate of 90.5% at 5°C and 0.3% at 25°C.
[0159] Comparative Example 3: The single melamine-formaldehyde resin wall material microcapsules had a rupture rate of 45.7% at 5°C and a rupture rate of 3.2% at 25°C.
[0160] 2.2 Validation of Phase Transition Temperature by Differential Scanning Calorimetry (DSC) The microcapsules were tested using a differential scanning calorimeter (model TAQ2000) with a temperature range of -10℃ to 30℃ and a heating rate of 2℃ / min.
[0161] Test results showed that all microcapsules exhibited significant endothermic peaks within the range of 5.6℃ to 5.9℃, corresponding to the liquid-solid phase transition initiation temperature of the core material, n-tetradecane. Since the phase transition is a continuous process, when the temperature dropped to 5℃, the phase transition of n-tetradecane was completely completed, with the volume expansion rate reaching its maximum value of 10% to 15%, generating sufficient local stress to cause the composite wall material to crack.
[0162] The above test results show that the temperature-reversible phase change microcapsules prepared in this application have excellent temperature response characteristics: they hardly break under normal temperature (25℃) storage conditions, which can ensure the long-term storage stability of component B; they can break rapidly and in large quantities under low temperature construction environment ≤5℃, releasing the highly active titanium-based co-catalyst encapsulated inside, thereby achieving low-temperature rapid curing of the sealant.
[0163] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of this application should be included within the protection scope of this application.
Claims
1. A two-component silicone structural sealant, characterized in that, The two-component silicone structural sealant comprises component A and component B; wherein... Component A comprises the following components in parts by weight: α,ω-dihydroxypolydimethylsiloxane, 90-110 parts; Reinforcing filler, 10-20 parts; Composite silane coupling agent, 1-3 parts; Component B comprises the following components in parts by weight: Silane crosslinking agent, 55-65 parts; Low-activity organic bismuth catalyst, 1-3 parts; Temperature-reversible phase change microcapsules, 10-20 parts; The temperature-reactive phase change microcapsule has a core-shell structure. The wall material of the temperature-reactive phase change microcapsule is a composite wall material of melamine-formaldehyde resin and polyurethane. The core material of the temperature-reactive phase change microcapsule includes n-tetradecane and a highly active titanium-based cocatalyst. The temperature-reactive phase change microcapsule can rupture and release the highly active titanium-based cocatalyst when the curing construction environment temperature is ≤5℃.
2. The two-component silicone structural sealant as described in claim 1, characterized in that, The composite silane coupling agent is a compound comprising an aminosilane coupling agent and an epoxysilane coupling agent.
3. The two-component silicone structural sealant as described in claim 1, characterized in that, The inverse temperature responsive phase change microcapsules have a particle size of 5μm to 10μm and a wall material thickness of 0.5μm to 1μm.
4. The two-component silicone structural sealant as described in claim 1, characterized in that, In the core material of the temperature-reversible phase change microcapsule, the mass ratio of n-tetradecane to the highly active titanium-based cocatalyst is 93~97:3~7.
5. The two-component silicone structural sealant as described in claim 1, characterized in that, The highly active titanium-based cocatalyst is diisopropyl di(acetylacetonyl)titanate.
6. A method for preparing a two-component silicone structural sealant as described in any one of claims 1 to 5, characterized in that, An application in a sealant preparation system, the sealant preparation system including a stirring execution module and a temperature control module, the method comprising: The α,ω-dihydroxypolydimethylsiloxane, the reinforcing filler, and the composite silane coupling agent are mixed evenly to obtain component A. The silane crosslinking agent and the low-activity organic bismuth catalyst were mixed evenly to obtain the basic system of component B. The n-tetradecane and the highly active titanium-based co-catalyst are mixed evenly to obtain the core material of the temperature-reversible phase change microcapsule; The core material is coated and cured using the melamine-formaldehyde resin and polyurethane composite wall material to obtain the temperature-reversible phase change microcapsules. The inverse temperature response phase change microcapsules are added to the B-component base system, stirred and dispersed, and the shear stress and temperature information of the B-component base system are obtained; wherein, the shear stress information is used to reflect the magnitude of the shear impact on the inverse temperature response phase change microcapsules during the dispersion process, and the temperature information is used to reflect the temperature fluctuation of the B-component base system during the dispersion process. The rotation speed of the stirring execution module is controlled based on the shear stress information, and the output power of the temperature control module is controlled based on the temperature information to obtain the uniformly dispersed component B. The A component and the B component are sealed and stored separately to obtain the two-component silicone structural sealant.
7. The method for preparing the two-component silicone structural sealant as described in claim 6, characterized in that, The method of controlling the rotational speed of the stirring execution module based on the shear stress information includes: Based on the wall material structure characteristics of the inverse temperature response phase change microcapsules, the upper limit threshold of the non-rupture shear stress of the inverse temperature response phase change microcapsules is determined. Based on the rheological properties of the B-component basic system, the effective dispersion shear stress lower limit threshold of the temperature-reversible phase change microcapsules was determined. Based on the upper limit threshold of the non-ruptured capsule shear stress and the lower limit threshold of the effective dispersed shear stress, the safe operating range of shear stress for the temperature-reversible phase change microcapsule is obtained. The measured value of shear stress is obtained based on the shear stress information; The measured value of shear stress is compared with the safe working range of shear stress to obtain the comparison result; The rotation speed of the stirring execution module is controlled based on the comparison results.
8. The method for preparing the two-component silicone structural sealant as described in claim 7, characterized in that, The process of obtaining the measured shear stress value based on the shear stress information includes: Based on the shear stress information, fluid shear action correlation parameters are obtained; Based on the rheological properties of the B-component basic system and the actual operating state of the stirring execution module, a parameter conversion correspondence is constructed. Based on the parameter conversion correspondence, the fluid shear action related parameters are subjected to directional analytical transformation to obtain the transformed fluid shear action related parameters. The parameters associated with the transformed fluid shearing action are standardized to obtain the measured value of the shear stress.
9. The method for preparing the two-component silicone structural sealant as described in claim 6, characterized in that, The control of the output power of the temperature control module based on the temperature information includes: Based on the temperature information, the correlation parameters of the overall thermal environment of the B-component basic system are obtained; Based on the correlation parameters, the continuous heat load properties of the B-component basic system, and the temperature tolerance characteristics of the inverse-temperature response phase change microcapsules, a power regulation benchmark for the temperature control module is established. Based on the dynamic change trend of the associated parameters and the power adjustment benchmark, determine the power control requirements that are suitable for the current distributed operating conditions. Based on the power regulation requirements, the output power of the temperature control module is controlled.
10. The method for preparing the two-component silicone structural sealant as described in claim 9, characterized in that, The step of establishing a power regulation benchmark for the temperature control module based on the correlation parameters, the continuous heat load properties of the B-component basic system, and the temperature tolerance characteristics of the inversion-response phase change microcapsules includes: Based on the temperature tolerance characteristics of the inverse temperature response phase change microcapsules, the temperature constraint range suitable for the B component base system is determined. Based on the continuous heat load properties of the B-component basic system, generate corresponding heat load constraints for the B-component basic system. Based on the correlation parameters, the temperature constraint range and the heat load constraint conditions are uniformly adapted and corrected to obtain the corrected composite constraint conditions. By integrating the modified composite constraints, the power regulation reference of the temperature control module is obtained.