CN112812737B - High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall - Google Patents

High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall Download PDF

Info

Publication number
CN112812737B
CN112812737B CN202110019501.4A CN202110019501A CN112812737B CN 112812737 B CN112812737 B CN 112812737B CN 202110019501 A CN202110019501 A CN 202110019501A CN 112812737 B CN112812737 B CN 112812737B
Authority
CN
China
Prior art keywords
parts
component
surface treatment
mass
airplane
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110019501.4A
Other languages
Chinese (zh)
Other versions
CN112812737A (en
Inventor
张东岳
叶李薇
罗淑文
曾皓翔
梅拥军
谢麟
孙传鹏
周洪
赵芯
李文艳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chengdu Newave Aerochemical Co ltd
Original Assignee
Chengdu Newave Aerochemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chengdu Newave Aerochemical Co ltd filed Critical Chengdu Newave Aerochemical Co ltd
Priority to CN202110019501.4A priority Critical patent/CN112812737B/en
Publication of CN112812737A publication Critical patent/CN112812737A/en
Application granted granted Critical
Publication of CN112812737B publication Critical patent/CN112812737B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213Oxides; Hydroxides of metals of rare earth metal of cerium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses an organic silicon sealant for high-temperature resistance and flame retardance of an airplane firewall, which consists of 10 parts of a component A and 1 part of a component B in parts by mass; the component A comprises the following components in parts by mass: 40 portions of monophenyl silica gel with 20 percent of phenyl content; 10 parts of basalt chopped yarn subjected to surface treatment by a water repellent; 20 parts of lanthanum oxide; 10 parts of cerium oxide; 5 parts of glass powder; 20 parts of mica powder modified by surface treatment; the component B comprises the following components in parts by mass: 5 parts of trisilicol ethyl esterification cage-shaped silsesquioxane; 4 parts of ethyl orthosilicate; dibutyl tin dilaurate, 0.2 parts. The organic silicon sealant can realize that flame at 1100 ℃ can not penetrate after being burnt for 30min, has excellent heat insulation performance, the back temperature of a titanium alloy plate is not more than 250 ℃, the back temperature of an aluminum alloy plate is not more than 200 ℃, and the tensile strength of the aluminum alloy plate after long-time heat aging is more than 5MPa.

Description

High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall
Technical Field
The invention belongs to the field of sealants, and relates to an organic silicon sealant for high-temperature resistance and flame retardance of an airplane firewall.
Technical Field
In order to isolate certain potentially flammable zones, protect places that may be subjected to extreme temperatures, the design of firewalls is required at the location of engines, auxiliary power plants, combustion igniters, etc. in aircraft, spacecraft and ships. Fire retardant silicone sealants are an indispensable material in firewall construction. The technical scheme at the present stage is that the flame-retardant material is prepared by adding flame-retardant filler, such as inorganic and organic flame retardants of aluminum hydroxide, platinum compounds, melamine and the like, and by a physical mixing method. However, with the progress of aerospace technology, the design has more outstanding requirements on the flame retardance and high temperature resistance of components, the working temperature of the original sealant (< 200 ℃) and the flame retardance cannot be sufficient (the flame combustion resisting time cannot exceed 15 min), and the development of aerospace vehicles is limited due to safety considerations. Therefore, the preparation of flame retardant sealants with better performance has great value.
Disclosure of Invention
In view of the above, the present invention provides a high temperature resistant and flame retardant silicone sealant for an aircraft firewall. The technical scheme is as follows:
1. an organic silicon sealant for high-temperature resistance and flame retardance of an airplane firewall comprises 10 parts of a component A and 1 part of a component B in parts by mass; the component A comprises the following components in parts by weight: 40 parts of monophenyl silica gel with the phenyl content being 20 percent; 10 parts of basalt chopped yarn subjected to surface treatment by a water repellent; 20 parts of lanthanum oxide; 10 parts of cerium oxide; 5 parts of glass powder; 20 parts of mica powder modified by surface treatment; the component B comprises the following components in parts by mass: 5 parts of trisilicitol ethyl esterification cage-shaped silsesquioxane; 4 parts of ethyl orthosilicate; dibutyl tin dilaurate, 0.2 parts.
Furthermore, the viscosity range of the monophenyl silica gel is 8000-20000cP.
Further, the length of the basalt chopped strand subjected to the surface treatment by the water repellent is 1.5cm.
Further, the preparation process of the basalt chopped strand after the surface treatment of the water repellent comprises the following steps: the continuous basalt filament is firstly drawn through a liquid tank filled with silane coupling agent, and then passes through a 10-meter drying tunnel dried by hot air at 80 ℃, wherein the silane coupling agent comprises KH550, KH560 and KH570.
Further, the preparation and modification process of the white mica powder modified by surface treatment comprises the following steps: adding 2000 mesh 100 parts of common muscovite powder into a vacuum kneader, diluting 3 parts of hexamethyldisilazane with 20 parts of ethanol, adding the hexamethyldisilazane into the vacuum kneader, heating and kneading at 120 ℃ for 15min, starting vacuum, keeping the vacuum degree less than 0.1mpa, and kneading for 2h to obtain the surface modified muscovite powder.
Further, the granularity of the glass powder is 6 μm.
Further, the cerium oxide is 1250 meshes.
Further, the preparation method of the component A comprises the following steps: adding phenyl silica gel, lanthanum oxide, cerium oxide and surface-treated modified muscovite powder into a double-planet high-speed mixer, stirring at 800rpm/min, vacuumizing for 30min to ensure that the vacuum degree is less than-0.1 mpa, stopping stirring, adding basalt fiber, stirring at less than 400rpm/min, vacuumizing for 15min to ensure that the vacuum degree is less than-0.1 mpa, and discharging.
Further, the preparation method of the component B comprises the following steps: adding trisiliconate ethyl ester polyhedral oligomeric silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, simultaneously keeping the vacuum degree less than-0.1 mpa, stirring for 10min, discharging and filling.
The invention has the beneficial effects that:
the component A adopts monophenyl silica gel with 20 percent of phenyl content, the viscosity range is 8000-20000cP, and high-heat-resistant resin plays the roles of bonding and sealing; the tensile strength, the bonding strength and the anti-cracking strength of the material in a limited hot oxygen environment can be improved by adding anti-cracking reinforcing fibers (basalt chopped yarns subjected to surface treatment by a water repellent); by adding a proper amount of rare earth elements, the compactness of the material and the binding force between the material and a matrix can be improved, the oxidation rate is reduced, and the anti-stripping performance of an oxidation film is improved, so that the high-temperature oxidation resistance of the material is obviously improved; the white mica is added into a porcelain material (surface treatment modified white mica powder), is a complex silicate, has a melting point of about 1800 ℃ or even higher, when the silicate filler is added, silicon dioxide generated by the decomposition of silicone rubber reacts with the silicate filler to form a eutectic mixture at the edge of the filler, the eutectic material can play a bridging role between silicon dioxide particles and filler particles to form a condensed ceramic product, the white mica is used as a porcelain material and is a ceramic continuous phase material which is subjected to ceramic transformation in high-temperature flame to form a hard continuous ceramic layer, the fire resistance of the material is improved, the white mica has better electrical insulation and fire resistance, but the strength of a sintered body at the high temperature of more than 1000 ℃ is not enough, the surface treatment modification is carried out to increase the interface compatibility of the white mica and a resin matrix, the ceramic continuous phase is better formed, and the strength at the high temperature is higher.
Adding rare earth elements which are positioned in IIIB group of the periodic table of elements and comprise 17 elements including scandium (So), yttrium (Y) and lanthanide elements (Ln). When the rare earth elements form compounds, all the 4f,5d,6S and 6p can be used as valence orbitals, valence electrons extend in multiple spatial directions, and compared with lead and barium only using the 6s and 6p as valence orbitals, the space coverage range of the valence electrons is larger, so that the probability of Compton scattering can be increased; in addition, the special 4f electron layer can realize multiple energy level transitions, and the harm of high-energy rays is weakened after a large amount of energy is consumed; therefore, rare earth elements have excellent absorption characteristics for low and medium energy rays. Therefore, the addition of the rare earth compound can effectively enhance the thermal oxygen stability and radiation resistance of the material.
The component B adopts a monophenyl silica gel structure instead of common dimethyl siloxane, and a crosslinking system is a POSS silsesquioxane structure, so that the composition has the advantages of high crosslinking density, high rigidity and high heat resistance.
The flame-retardant plugging material can realize that flame at 1100 ℃ can not penetrate after being burnt for 30min, has excellent heat-insulating property, the back temperature of the titanium alloy plate is not more than 250 ℃, the back temperature of the aluminum alloy plate is not more than 200 ℃, and the tensile strength is more than 5MPa after long-time heat aging.
Detailed Description
The following describes preferred embodiments of the present invention in detail.
Example 1
A flame-retardant high-temperature-resistant sealant capable of being ceramized comprises, by mass, 10 parts of a component A and 1 part of a component B;
the component A is as follows: 40 portions of monophenyl silica gel (the viscosity range is 8000-20000 cP) with the phenyl content of 20 percent; the basalt chopped strand is subjected to surface treatment by a water repellent, the length of the basalt chopped strand is 1.5cm, and 10 parts of the basalt chopped strand is prepared (the preparation process of the basalt chopped strand subjected to surface treatment by the water repellent comprises the steps of firstly drawing continuous basalt long fibers through a liquid tank containing a silane coupling agent, then passing through a 10-meter drying tunnel dried by hot air at 80 ℃, wherein the silane coupling agent comprises KH550, KH560, KH570 and the like); 800 meshes of lanthanum oxide and 20 meshes of cerium oxide, and 1250 meshes of cerium oxide; 5 parts of glass powder with the particle size of 6 microns; 20 parts of surface-treated and modified muscovite powder (the surface-treated and modified muscovite powder is prepared and modified by adding 2000 meshes of common muscovite powder into a vacuum kneader, diluting 3 parts of hexamethyldisilazane with 20 parts of ethanol, adding the hexamethyldisilazane into the vacuum kneader, heating and kneading at 120 ℃ for 15min, starting vacuum, keeping the vacuum degree less than 0.1mpa, and kneading for 2h to obtain the surface-modified muscovite powder).
The preparation method of the component A comprises the following steps: in a double planetary high-speed mixer, firstly adding phenyl silica gel, then adding rare earth compound, forming porcelain material, high-speed stirring (> 800 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 30min, then stopping stirring, adding basalt fiber, low-speed stirring (< 400 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 15min, and discharging.
The component B is as follows: 5 parts of trisilicol ethyl esterification cage-shaped silsesquioxane; 5 parts of ethyl orthosilicate; 0.2 part of dibutyltin dilaurate;
the preparation method of the component B comprises the following steps: adding trisiliconate ethyl ester polyhedral oligomeric silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, and simultaneously keeping the vacuum degree less than-0.1 mpa. Stirring for 10min, discharging, and bottling.
Comparative example 1
In the comparative example, on the basis of the embodiment 1, the basalt fiber is replaced by the kaolin, so that the ceramic fiber has the ceramic property and does not have the toughening and anti-cracking effects. Can vitrify and resist high temperature, but the mechanical property after high temperature is poor, the concrete formulation is:
consists of 10 parts of component A and 1 part of component B;
the component A is as follows: the component A is as follows: 40 portions of monophenyl silica gel with 20 percent of phenyl content, the viscosity range is 8000-20000cP; 10 parts of kaolin 800 meshes, silicon micropowder, calcium carbonate, quartz sand, alumina and the like; 800 meshes of lanthanum oxide and 20 meshes of cerium oxide, and 1250 meshes of cerium oxide; 5 parts of glass powder with the particle size of 6 microns; 20 parts of surface-treated and modified muscovite powder (the surface-treated and modified muscovite powder is prepared and modified by the following steps of adding 2000 meshes of common muscovite powder into a vacuum kneader, diluting 3 parts of hexamethyldisilazane with 20 parts of ethanol, adding the hexamethyldisilazane into the vacuum kneader, heating and kneading at 120 ℃ for 15min, starting vacuum, keeping the vacuum degree below 0.1mpa, and kneading for 2h to obtain the surface-modified muscovite powder).
The preparation method of the component A comprises the following steps: in a double planetary high-speed mixer, firstly adding phenyl silica gel, then adding rare earth compound, forming porcelain material, high-speed stirring (> 800 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 30min, then stopping stirring, adding basalt fiber, low-speed stirring (< 400 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 15min, and discharging.
The component B is as follows: 5 parts of trisilicol ethyl esterification cage-shaped silsesquioxane; 5 parts of ethyl orthosilicate; 0.2 part of dibutyltin dilaurate;
the preparation method of the component B comprises the following steps: adding trisilicol ethyl esterification cage-shaped silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, and simultaneously keeping the vacuum degree less than-0.1 mpa. Stirring for 10min, discharging, and bottling.
Comparative example 2
In the comparative example, on the basis of the embodiment 1, the modified mica is replaced by the common mica, so that the vitrification effect is poor, and the high-temperature resistance is reduced. The specific formula is as follows: consists of 10 parts of component A and 1 part of component B;
the component A is as follows: 40 portions of monophenyl silica gel with 20 percent of phenyl content, the viscosity range is 8000-20000cP; 10 parts of basalt chopped strand with the length of 1.5 cm; 800 meshes of lanthanum oxide and 20 meshes of cerium oxide, and 1250 meshes of cerium oxide; 5 parts of glass powder with the particle size of 6 microns; the common muscovite powder is 2000 meshes and 20 parts.
The preparation method of the component A comprises the following steps: in a double-planet high-speed mixer, firstly adding phenyl silica gel, then adding rare earth compound and ceramic forming material, high-speed stirring (> 800 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 30min, then stopping stirring, adding basalt fiber, low-speed stirring (< 400 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 15min, and discharging.
The component B is as follows: 5 parts of trisilicol ethyl esterification cage-shaped silsesquioxane; 5 parts of ethyl orthosilicate; 0.2 part of dibutyltin dilaurate;
the preparation method of the component B comprises the following steps: adding trisilicol ethyl esterification cage-shaped silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, and simultaneously keeping the vacuum degree less than-0.1 mpa. Stirring for 10min, discharging and filling.
Comparative example 3
In the comparative example, on the basis of the implementation 1, trisilicol ethyl esterification cage-like silsesquioxane (POSS) in the component B is removed, the POSS has the function of inorganic and organic hybrid rigid toughening crosslinking network, the heat resistance stability and the mechanical property of the molecular framework are improved, and the heat resistance stability and the mechanical property are obviously reduced after the POSS is removed, and the specific formula is as follows:
consists of 10 parts of component A and 1 part of component B;
the component A is as follows: 40 portions of monophenyl silica gel with 20 percent of phenyl content, the viscosity range is 8000-20000cP; 1.5cm of basalt chopped yarn is subjected to surface treatment by a water repellent (10 parts of basalt continuous long fiber is firstly pulled to pass through a liquid tank containing a silane coupling agent, and then passes through a 10-meter drying tunnel dried by hot air at 80 ℃, wherein the silane coupling agent comprises 550 560 570 and the like); 800 meshes of lanthanum oxide and 20 meshes of cerium oxide, and 1250 meshes of cerium oxide; 5 parts of glass powder with the particle size of 6 microns; 20 parts of surface-treated and modified muscovite powder (the surface-treated and modified muscovite powder is prepared by the following steps of adding 2000 meshes of common muscovite powder to 100 parts of vacuum kneader, diluting 3 parts of hexamethyldisilazane with 20 parts of ethanol, adding the hexamethyldisilazane into the vacuum kneader, heating and kneading at 120 ℃ for 15min, starting vacuum, keeping the vacuum degree less than 0.1mpa, kneading for 2h to obtain the surface-modified muscovite powder)
The preparation method of the component A comprises the following steps: in a double-planet high-speed mixer, firstly adding phenyl silica gel, then adding rare earth compound and ceramic forming material, high-speed stirring (> 800 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 30min, then stopping stirring, adding basalt fiber, low-speed stirring (< 400 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 15min, and discharging.
The component B is as follows: 10 parts of ethyl orthosilicate; 0.2 part of dibutyltin dilaurate;
the preparation method of the component B comprises the following steps: adding trisilicol ethyl esterification cage-shaped silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, and simultaneously keeping the vacuum degree less than-0.1 mpa. Stirring for 10min, discharging and filling.
Comparative example 4
In the comparative example, on the basis of the embodiment 1, lanthanum oxide and cerium oxide are replaced by high-purity silicon micropowder, so that the thermal-oxidative aging resistance and the high-temperature resistance are greatly reduced. The specific formula is as follows:
consists of 10 parts of component A and 1 part of component B;
the component A is as follows:
40 portions of monophenyl silica gel (the viscosity range is 8000-20000 cP) with 20 percent of phenyl content;
the basalt chopped strand is subjected to surface treatment by a water repellent, the length of the basalt chopped strand is 1.5cm, and 10 parts of the basalt chopped strand is prepared (the preparation process of the basalt chopped strand subjected to surface treatment by the water repellent comprises the steps of firstly drawing continuous basalt long fibers through a liquid tank containing a silane coupling agent, then passing through a 10-meter drying tunnel dried by hot air at 80 ℃, wherein the silane coupling agent comprises KH550, KH560, KH570 and the like);
high-purity silicon micropowder 800 meshes, 30 parts;
5 parts of glass powder with the particle size of 6 microns;
20 parts of white mica powder modified by surface treatment (the preparation and modification process of the white mica powder modified by surface treatment comprises the steps of adding 2000 meshes of common white mica powder to 100 parts of vacuum kneader, diluting 3 parts of hexamethyldisilazane with 20 parts of ethanol, adding the mixture to the vacuum kneader, heating and kneading at 120 ℃ for 15min, starting vacuum, keeping the vacuum degree less than 0.1mpa, kneading for 2h to obtain the surface-modified white mica powder)
The preparation method of the component A comprises the following steps: in a double-planet high-speed mixer, firstly adding phenyl silica gel, then adding rare earth compound and ceramic forming material, high-speed stirring (> 800 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 30min, then stopping stirring, adding basalt fiber, low-speed stirring (< 400 rpm/min) and vacuumizing (vacuum degree < -0.1 mpa) for 15min, and discharging.
The component B is as follows: 5 parts of trisilicol ethyl esterification cage-shaped silsesquioxane; 5 parts of ethyl orthosilicate; 0.2 part of dibutyltin dilaurate;
the preparation method of the component B comprises the following steps: adding trisiliconate ethyl acetate polyhedral oligomeric silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, and simultaneously keeping the vacuum degree to be less than-0.1 mpa. Stirring for 10min, discharging and filling.
The materials obtained in the examples and comparative examples were subjected to mechanical property, thermal aging resistance and burn-through resistance test to obtain the results shown in table 1.
According to the requirements of flame penetration test method of the sealant of the aerospace firewall in accordance with the international aviation standard SAE AS 5127/2, the sealant obtained in the embodiment and the comparative example is coated on an aluminum alloy base material, and is burned for 30min by using flame at 1100 ℃, so AS to verify whether the performance requirements of the aerospace firewall part can be met.
TABLE 1 comparison table of mechanics, thermal aging resistance and burn-through resistance
Figure BDA0002887975430000061
Figure BDA0002887975430000071
As can be seen from table 1:
the mechanical properties of the anti-cracking component basalt fiber reinforced material in high-temperature and radiation environments are added, particularly in a high-temperature combustion environment, the material has excellent shock resistance and anti-cracking performance after ceramic phase transformation, and the problem of large brittleness of the traditional ceramic silicon rubber material after ceramic formation is solved;
the mica which is a ceramic forming material is modified, so that the interface compatibility is improved, the ceramic forming efficiency is higher, the surface of the material is smooth and compact, and the mechanical property is more excellent.
The molecular structure of POSS contains Si-like 0 2 And when the component A and the component B are mixed, vulcanized and cured, silane on the POSS and hydroxyl on phenyl silicon are crosslinked, so that a cured product containing a POSS cage structure is obtained, and the heat resistance, oxidation resistance, flame retardance and other properties of the sealant can be improved.
The rare earth compound is used for improving the thermal oxidation aging property and the radiation resistance of the material, and the high temperature resistance and the radiation resistance of the material are greatly enhanced.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.

Claims (8)

1. The organic silicon sealant for the high-temperature resistance and flame retardance of the fire wall of the airplane is characterized by comprising 10 parts of a component A and 1 part of a component B in parts by mass; the component A comprises the following components in parts by mass: 40 portions of monophenyl silica gel with 20 percent of phenyl content; 10 parts of basalt chopped yarn subjected to surface treatment by a water repellent; 20 parts of lanthanum oxide; 10 parts of cerium oxide; 5 parts of glass powder; 20 parts of mica powder modified by surface treatment; the component B comprises the following components in parts by mass: 5 parts of trisilicitol ethyl esterification cage-shaped silsesquioxane; 4 parts of ethyl orthosilicate; 0.2 part of dibutyltin dilaurate; the monophenyl silica gel contains hydroxyl.
2. The silicone sealant as claimed in claim 1, wherein the viscosity of the single phenyl silicone gel is 8000-20000cP.
3. The silicone sealant for high temperature resistance and flame retardance of aircraft firewalls as claimed in claim 1, wherein said water repellent surface treated basalt chopped strand is 1.5cm in length.
4. The high-temperature-resistant flame-retardant silicone sealant for the airplane firewall according to claim 1, wherein the basalt chopped strand subjected to the surface treatment by the water repellent is prepared by the following steps: the continuous basalt filament is firstly drawn through a liquid tank filled with silane coupling agent, and then passes through a 10-meter drying tunnel dried by hot air at 80 ℃, wherein the silane coupling agent comprises KH550, KH560 and KH570.
5. The silicone sealant for high temperature resistance and flame retardance of aircraft firewalls according to claim 1, wherein the surface-treated and modified muscovite powder is prepared and modified by the following steps: adding 2000 mesh 100 parts of common muscovite powder into a vacuum kneader, diluting 3 parts of hexamethyldisilazane with 20 parts of ethanol, adding the hexamethyldisilazane into the vacuum kneader, heating and kneading at 120 ℃ for 15min, starting vacuum, keeping the vacuum degree less than 0.1mpa, and kneading for 2h to obtain the surface modified muscovite powder.
6. The silicone sealant according to claim 1, wherein the glass frit has a particle size of 6 μm.
7. The silicone sealant according to claim 1, wherein the cerium oxide is 1250 mesh.
8. The high-temperature-resistant flame-retardant silicone sealant for the fire wall of the airplane as claimed in claim 1, wherein the preparation method of the component B comprises the following steps: adding trisiliconate ethyl acetate polyhedral oligomeric silsesquioxane, ethyl orthosilicate and dibutyltin dilaurate into a reaction kettle, starting stirring, keeping the vacuum degree below-0.1 mpa, stirring for 10min, discharging and filling.
CN202110019501.4A 2021-01-07 2021-01-07 High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall Active CN112812737B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110019501.4A CN112812737B (en) 2021-01-07 2021-01-07 High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110019501.4A CN112812737B (en) 2021-01-07 2021-01-07 High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall

Publications (2)

Publication Number Publication Date
CN112812737A CN112812737A (en) 2021-05-18
CN112812737B true CN112812737B (en) 2022-11-25

Family

ID=75868713

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110019501.4A Active CN112812737B (en) 2021-01-07 2021-01-07 High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall

Country Status (1)

Country Link
CN (1) CN112812737B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008266609A (en) * 2007-03-22 2008-11-06 Nippon Shokubai Co Ltd Transparent resin composition and cured product thereof
CN104726054A (en) * 2015-04-10 2015-06-24 哈尔滨工业大学 Low expansion high temperature adhesive and preparation method thereof
CN106350001A (en) * 2016-10-09 2017-01-25 广州集泰化工股份有限公司 Organic silicon sealant capable of being ceramized at high temperature and preparation method of organic silicon sealant
CN109021912A (en) * 2018-06-21 2018-12-18 中国民用航空总局第二研究所 A kind of aircraft environmental protection type sealing adhesive and preparation method thereof
CN111286121A (en) * 2020-03-09 2020-06-16 上海古太创意服务有限公司 Antibacterial protection environment-friendly composite polymer material and preparation method and application thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2843134B1 (en) * 2002-07-30 2006-09-22 Ferrari S Tissage & Enduct Sa METHOD FOR TREATING IMPREGNATION OF ARCHITECTURAL TEXTILES BY A SILICONE COMPOSITION CROSSLINKED IN ELASTOMER AND ARCHITECTURAL TEXTILE SO COATED

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008266609A (en) * 2007-03-22 2008-11-06 Nippon Shokubai Co Ltd Transparent resin composition and cured product thereof
CN104726054A (en) * 2015-04-10 2015-06-24 哈尔滨工业大学 Low expansion high temperature adhesive and preparation method thereof
CN106350001A (en) * 2016-10-09 2017-01-25 广州集泰化工股份有限公司 Organic silicon sealant capable of being ceramized at high temperature and preparation method of organic silicon sealant
CN109021912A (en) * 2018-06-21 2018-12-18 中国民用航空总局第二研究所 A kind of aircraft environmental protection type sealing adhesive and preparation method thereof
CN111286121A (en) * 2020-03-09 2020-06-16 上海古太创意服务有限公司 Antibacterial protection environment-friendly composite polymer material and preparation method and application thereof

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
BFRP筋与玄武岩纤维再生混凝土黏结性能试验研究;刘华新等;《混凝土》;20151227(第12期);第101-104页 *
Thermal stability enhancement mechanism of poly(dimethylsiloxane) composite by incorporating octavinyl polyhedral oligomeric silsesquioxanes;Yang, D等;《POLYMER DEGRADATION AND STABILITY 》;20130630;第98卷(第1期);第109-114页 *
氧化锆对炭纤维增强耐烧蚀复合材料烧蚀性能的影响;刘艳辉等;《固体火箭技术》;20160415(第02期);第119-122、128页 *
耐高温室温固化有机硅胶粘剂的合成与表征;葛铁军等;《中国胶粘剂》;20171231(第10期);第20-24页 *
耐高温有机硅粘接剂的研究新进展;岳远志等;《有机硅材料》;20101125;第24卷(第06期);第56-61页 *
聚有机硅倍半氧烷热解研究进展;马军等;《高分子通报》;20011030(第05期);第36-40页 *
航空双组分密封胶适航与验证技术研究;叶李薇等;《化工新型材料》;20200715(第07期);第244-249页 *

Also Published As

Publication number Publication date
CN112812737A (en) 2021-05-18

Similar Documents

Publication Publication Date Title
CN101747631B (en) Flame-retardant room temperature vulcanized silicone rubber composition
CN111378285B (en) High-strength high-flame-retardant organic silicon foam material and preparation method thereof
CN109401634B (en) Flame-retardant smoke-inhibiting ceramizable room temperature vulcanized organosilicon sealant and preparation method thereof
CN113136140B (en) Organic silicon fireproof heat-insulating coating and preparation method thereof
CN113476777B (en) Rope-shaped temperature-sensitive microcapsule non-pressure fire extinguishing material and preparation method thereof
CN110845850B (en) Ceramizable halogen-free flame-retardant silicone rubber and preparation method thereof
CN108219473A (en) Room temperature vulcanization Ceramic silicon rubber foam seal agent and preparation method thereof
CN111500071A (en) Single-component flame-retardant silica gel foam material and preparation method thereof
CN112500789A (en) Fireproof heat-insulating coating for delaying thermal diffusion of lithium battery and preparation method thereof
CN114409997A (en) High-flame-retardance photoelectric composite cable sheath material with good processability and preparation method thereof
CN110713725A (en) Ceramic silicon rubber composite insulating cable material
CN114106767A (en) Low-specific-gravity fireproof silicone sealant and preparation method thereof
CN115595114B (en) High-displacement flame-retardant silicone sealant and preparation method thereof
CN110643183A (en) Fire-resistant silicone rubber and preparation method thereof
CN117487509A (en) Ceramic flame-retardant fireproof silicone sealant
CN112812737B (en) High-temperature-resistant flame-retardant organic silicon sealant for airplane firewall
CN114763459A (en) High-toughness thermal-aging-resistant fluorescent sizing material after curing
CN110396297B (en) Fireproof high-temperature-resistant organic silicon rubber material and preparation method thereof
CN106317964A (en) Submicron composite sphere and preparation method thereof, and application of submicron composite sphere as silicone rubber ceramic-forming filling material
CN114605839B (en) Ceramic silicon rubber with obvious XRD new crystallization peak after calcination and preparation method thereof
CN116515299A (en) Ceramic silicon rubber composite material and preparation method and application thereof
CN115717052A (en) Graphene modified single-component sealant capable of resisting high temperature for long time and preparation method and application thereof
CN115093826A (en) High-thermal-conductivity low-specific-gravity adhesive and preparation method thereof
CN110305368A (en) It is flame-retardant expanded dose a kind of and its preparation method and application
CN112300445A (en) Ceramic refractory filler and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant