CN111253860A - Ablation-resistant organic silicon resin coating material and preparation method thereof - Google Patents
Ablation-resistant organic silicon resin coating material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions 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; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
An ablation-resistant organic silicon resin coating material and a preparation method thereof. The ablation-resistant organic silicon resin coating material comprises octaglycidyl ether oxypropyl POSS, aminopropyl triethoxysilane, dibutyltin dilaurate and hydroxyl-terminated polydimethylsiloxane. According to the invention, coating materials with different ablation resistance can be obtained by changing the addition amount of the cross-linking agent, POSS is taken as the cross-linking agent to cure the organic silicon resin at room temperature, and the core of the organic silicon resin is that epoxy groups at the periphery of glycidyl ether oxypropyl POSS and primary amine groups at the chain end of aminopropyltriethoxysilane have extremely high reaction activity, so that the epoxy groups and the primary amine groups are easy to undergo a ring-opening addition reaction. The invention can avoid the serious agglomeration of the cross-linking agent, improve the tensile strength and the ablation resistance of the organic silicon resin material, and save the process cost by room-temperature forming.
Description
Technical Field
The invention relates to the field of thermal protection of solid rocket engines, in particular to a method capable of improving ablation resistance of an organic silicon resin coating.
Background
24 months 4 and 24 days 1970, the first satellite in China, eastern Red first, was successfully launched, which marked that China became the fifth aerospace big country capable of manufacturing and launching satellites in the United states, Su, Fa, and the fourth Japan. China is one of the world aerospace strong countries nowadays, from flying by people for the first time to Chang' e flying to the moon, the aerospace technology of China is continuously developed in recent years, so that the national defense strength is remarkably improved, and the civil infrastructure is further consolidated. Nowadays, in order to accelerate the realization of the comprehensive exploration of a distant galaxy, a spacecraft needs to achieve the aim of 'flying faster and flying farther', which brings challenges to the cruising ability of the spacecraft. The on-orbit continuous work of various spacecrafts can not leave the normal operation of the high-thrust carrier rocket. For a solid propulsion system, the propulsion device is a core device mainly comprising a solid rocket engine. In pursuit of higher payload, ramjet engines have now been developed that utilize oxygen in the air as one of the oxidants, both of which are widely used in the domestic and aerospace fields. The insulation between the engine and the outer casing plays a critical role. When the rocket engine runs, the temperature generated by the combustion of the propellant is up to 3000 ℃, and the heat insulation material is in direct contact with high-temperature and high-pressure fuel gas during the period, so that the rocket engine does not lose strength and burn through, and the continuous and safe running of the rocket body is ensured. The heat insulating material adopted in China at present mainly comprises a resin-based composite material (phenolic resin) and a flexible elastomer composite material (nitrile rubber, ethylene propylene diene monomer rubber and silicone rubber). Resin-based composite materials, although having more excellent thermal stability than elastomer heat insulating materials, are highly susceptible to thermal expansion at high temperatures and pressures, which is detrimental to the protection of the housing. Silicon-based ablation-resistant composites are widely used in ramjet engines because silicone rubber is composed of a Si-O structure with higher bond energy and has relatively better thermal stability. The performance of the matrix influences the overall performance of the composite material, but the unreinforced silicone rubber matrix has poor mechanical properties; is inflammable when exposed to open fire; the ablation rate is high at high temperature, and the reinforced organosilicon material has to be vulcanized and molded at high temperature, which brings high production cost for practical application.
POSS is used as a multifunctional organic/inorganic nano material, the exterior of the POSS has reactive or non-reactive groups, the reactive groups can realize the chemical bonding effect between the POSS and polymers, and the non-reactive groups can improve the compatibility between the POSS and the polymers. The POSS composite polymer material solves the problems of poor dispersibility, difficult processing and the like of common nano materials in polymers, and the mechanical property and the thermal stability of a modified system can be enhanced by doping the POSS composite polymer material. However, the physical blending of POSS into polymer systems requires a sacrifice in mechanical properties to slightly improve the ablation resistance of the material, but this method requires a large amount of POSS, and therefore the production cost is high.
In the early days, POSS entered into polymer matrix mainly in a physical blending way without any chemical reaction with the matrix and filler, wherein octaphenyl POSS and octaaminophenyl POSS are superior to other functional POSS in thermal stability, and are often used as the first filler for modifying polymer. The addition of octaphenyl POSS to phenolic resin is reported in International journal RSC advances in 2015, volume 5, 12, 8757, 8769, and the results show that the addition of POSS to a polymer matrix in a physical blending manner improves the ablation resistance of the material to some extent, but the POSS molecules existing in the polymer in a free state are easy to agglomerate, possibly affecting the crosslinking degree or the mechanical property of the system. Subsequent research has focused on chemically bonding POSS to polymer matrices to improve the ablation resistance of composites, including polyurethane, epdm, silicone rubber, and the like. In 2019, volume 42, page 717-723, the solid rocket technology reports that a small amount of methacryloxypropyl POSS and ethylene propylene diene monomer are reacted at high temperature and high pressure to obtain a modified heat-insulating material, the POSS can be introduced into a polymer system as a grafting agent through the reaction of alkenyl groups on the periphery of the POSS and alkenyl groups on a rubber main chain, and the mechanical property and the ablation resistance of the material are improved. Compared with physical blending, chemical bonding can produce relatively remarkable effect when improving comprehensive performance, but part of POSS is easy to cause chemical agglomeration reaction among particles when being bonded with polymers, the situation is generally existed in most heat insulation systems, serious agglomeration among the POSS particles is probably promoted, and meanwhile, the material is required to be formed at high temperature and high pressure, and the industrial production cost is higher.
Disclosure of Invention
In order to overcome the defects that chemical agglomeration reaction among filler particles is easy to generate during POSS and polymer grafting reaction in the prior art and high industrial cost is brought by a high-temperature high-pressure production process in practical application, the invention provides an ablation-resistant organic silicon resin coating material crosslinked by POSS at room temperature and a preparation method thereof.
The ablation-resistant organic silicon resin coating material comprises 0.8-1.4 parts by mass of octaglycidyl ether oxypropyl POSS, 0.22-1.76 parts by mass of aminopropyl triethoxysilane, 0.1-0.5 parts by mass of dibutyltin dilaurate and 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane.
The molecular weight of the hydroxyl-terminated polydimethylsiloxane is 45000g & mol-1。
The specific process for preparing the ablation-resistant organic silicon resin coating material provided by the invention comprises the following steps:
step 1, constructing an inert gas protective atmosphere;
step 2, preparing a cross-linking agent;
when the cross-linking agent is prepared, 0.8-1.4 parts by mass of octaglycidyl ether oxypropyl POSS and 0.22-1.76 parts by mass of aminopropyltriethoxysilane are poured into a flask and then uniformly mixed in a nitrogen atmosphere to obtain a mixed liquid. And heating and stirring the obtained mixed liquid at the temperature of 60-80 ℃ and the speed of 600r/min for 10-25 min to obtain the colorless transparent oily liquid cross-linking agent with POSS as a core structure.
And 3, mixing the raw materials.
And mixing the obtained cross-linking agent with 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane, and uniformly stirring at room temperature at 800r/min to obtain a mixture. The resulting mixture was sonicated at 150W power for 30min to facilitate dispersion of the crosslinker. And adding 0.1-0.5 part by mass of dibutyltin dilaurate catalyst into the mixture subjected to ultrasonic treatment, uniformly stirring at the rotating speed of 800r/min, and performing ultrasonic treatment for 5min at the power of 150W. And (4) obtaining a mixture after the mixing is finished.
And 4, curing.
And (4) placing the mixture obtained in the step (3) in a vacuum oven. The vacuum box was evacuated to 0.85MPa and held for 5min to remove air bubbles from the mixture.
And curing the mixture subjected to bubble removal for 4-8 hours at room temperature to obtain the ablation-resistant organic silicon resin coating material.
The linear ablation rate of the ablation-resistant organic silicon resin coating material is 0.38-0.47 mm · s-1The mass ablation rate is 0.13 to 0.17g · s-1The tensile strength is 0.36 to 0.75 MPa.
The POSS crosslinking agent provided by the invention has high reaction activity, and the ablation resistance of the modified organic silicon resin coating is obviously improved.
The ablation-resistant organic silicon resin coating material provided by the invention is obtained by curing organic silicon resin at room temperature by using POSS as a cross-linking agent, and has the core that epoxy groups on the periphery of glycidol ether oxypropyl POSS and primary amine groups at the chain end of aminopropyltriethoxysilane have extremely high reaction activity, so that ring-opening addition reaction is easily generated between the epoxy groups and the primary amine groups. When the alkoxy group at the periphery of the material obtained after the reaction and the terminal hydroxyl group of the organic silicon resin are subjected to crosslinking reaction, POSS is smoothly introduced into the polymer in a chemical bonding mode. Compared with high-temperature vulcanization, the method not only reduces the industrial cost caused by high-temperature and high-pressure vulcanization, but also improves the mechanical strength and the ablation resistance of the organic silicon resin. The data of the embodiment shows that the tensile strength of the ablation-resistant silicone coating material provided by the invention is improved from 0.26MPa of pure silicone to 0.36 MPa-0.75 MPa, and the linear ablation rate is 0.47mm · s-1～0.38mm·s-1The mass ablation rate is 0.17 g.s-1～0.13g·s-1。
The organosilicon material prepared by the invention can be cured at room temperature, and has certain mechanical strength and ablation resistance. By changing the addition amount of the cross-linking agent, coating materials with different ablation resistance can be obtained. Compared with the traditional high-temperature vulcanized silicone material, the POSS is used as a cross-linking agent, the alkoxy of the POSS is condensed with the hydroxyl at the chain end of the room-temperature vulcanized silicone rubber, the chemical bonding of the POSS and the polymer is realized, the energy efficiency is realized, the serious agglomeration of the cross-linking agent is avoided, the tensile strength and the ablation resistance of the silicone resin material are improved, and the process cost is saved by room-temperature molding.
Detailed Description
The invention relates to an ablation-resistant organic silicon resin coating material taking POSS (polyhedral oligomeric silsesquioxane) as a cross-linking agent, which comprises 0.8-1.4 parts by mass of octaglycidyl ether oxypropyl POSS, 0.22-1.76 parts by mass of aminopropyltriethoxysilane, 0.1-0.5 part by mass of dibutyltin dilaurate and 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane.
The octaglycidyl ether oxypropyl POSS was purchased from Hybrid Plastics, USA, as a colorless, transparent oily liquid. The aminopropyltriethoxysilane is purchased from Jiangsu Huaian and Yuan chemical Co., Ltd, is colorless transparent liquid and is analytically pure. The dibutyltin dilaurate is purchased from Guangdong chemical reagent engineering technology research and development center, is colorless and transparent liquid, and is analytically pure. The hydroxyl-terminated polydimethylsiloxane is purchased from Shanghai resin factory, is a colorless transparent liquid, and has a molecular weight of 45000g & mol-1。
Components of the examples of the invention
The invention also provides a method for preparing the ablation-resistant organic silicon resin coating material, which comprises the following specific steps:
step 1, constructing an inert gas protective atmosphere.
A latex tube is used for connecting a nitrogen bottle with a cleaned and dried 50ml three-neck flask, and after a valve of the gas bottle is opened, nitrogen is continuously introduced for 15min to remove air in the bottle.
And 2, preparing a cross-linking agent.
Pouring 0.8-1.4 parts by mass of octaglycidyl ether oxypropyl POSS and 0.22-1.76 parts by mass of aminopropyltriethoxysilane into a flask, and uniformly mixing in a nitrogen atmosphere to obtain a mixed liquid. And heating and stirring the obtained mixed liquid at the temperature of 60-80 ℃ and the speed of 600r/min for 10-25 min to obtain the colorless transparent oily liquid cross-linking agent with POSS as a core structure.
And 3, mixing the raw materials.
And mixing the obtained cross-linking agent with 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane, and uniformly stirring at room temperature at 800r/min to obtain a mixture. The resulting mixture was sonicated at 150W power for 30min to facilitate dispersion of the crosslinker. And adding 0.1-0.5 part by mass of dibutyltin dilaurate catalyst into the mixture subjected to ultrasonic treatment, uniformly stirring at the rotating speed of 800r/min, and performing ultrasonic treatment at the power of 150W for 5min to obtain a mixture after mixing.
And 4, curing.
And (4) placing the mixture obtained in the step (3) in a vacuum oven. The vacuum box was evacuated to 0.85MPa and held for 5min to remove air bubbles from the mixture.
And curing the mixture subjected to bubble removal for 4-8 hours at room temperature to obtain the ablation-resistant organic silicon coating material taking POSS as a cross-linking agent.
The linear ablation rate and the mass ablation rate of the obtained ablation-resistant organic silicon coating material are respectively 0.47mm & s-1And 0.17g · s-1The tensile strength was 0.36 MPa.
The preparation process of 5 embodiments proposed by the invention is the same.
The different process parameters for preparing the cross-linking agent in each example are:
test parameters of the examples
Claims (5)
1. An ablation-resistant organic silicon resin coating material is characterized by comprising 0.8-1.4 parts by mass of octaglycidyl ether oxypropyl POSS, 0.22-1.76 parts by mass of aminopropyl triethoxysilane, 0.1-0.5 parts by mass of dibutyltin dilaurate and 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane.
2. The ablation-resistant silicone resin coating material of claim 1, wherein the hydroxyl-terminated polydimethylsiloxane has a molecular weight of 45000 g-mol-1。
3. A method for preparing the ablation-resistant silicone resin coating material of claim 1, which is characterized by comprising the following specific steps:
step 1, constructing an inert gas protective atmosphere;
step 2, preparing a cross-linking agent;
and 3, mixing the raw materials:
mixing the obtained cross-linking agent with 30-60 parts by mass of hydroxyl-terminated polydimethylsiloxane, and keeping the mixture at room temperature
Stirring uniformly at 800r/min to obtain a mixture; subjecting the resulting mixture to ultrasonication at a power of 150W for 30min to promote dispersion of the crosslinking agent; adding 0.1-0.5 part by mass of dibutyltin dilaurate catalyst into the mixture subjected to ultrasonic treatment, uniformly stirring at the rotating speed of 800r/min, and performing ultrasonic treatment for 5min under the power of 150W; mixing to obtain a mixture;
and 4, curing:
placing the mixture obtained in the step 3 in a vacuum oven; vacuumizing the vacuum box to 0.85MPa and maintaining
Holding for 5min to remove bubbles in the mixture;
and curing the mixture subjected to bubble removal for 4-8 hours at room temperature to obtain the ablation-resistant organic silicon resin coating material.
4. The method for preparing the ablation-resistant silicone resin coating material according to claim 3, wherein in the step of preparing the cross-linking agent, 0.8-1.4 parts by mass of octaglycidyl ether oxypropyl POSS and 0.22-1.76 parts by mass of aminopropyltriethoxysilane are poured into a flask and then uniformly mixed in a nitrogen atmosphere to obtain a mixed liquid; and heating and stirring the obtained mixed liquid at the temperature of 60-80 ℃ and the speed of 600r/min for 10-25 minutes to obtain the colorless transparent oily liquid cross-linking agent with POSS as a core structure.
5. The method for producing an ablation-resistant silicone resin coating material according to claim 1, wherein the ablation-resistant silicone resin coating material has a linear ablation rate of 0.38 to 0.47mm · s-1The mass ablation rate is 0.13 to 0.17g · s-1The tensile strength is 0.36 to 0.75 MPa.
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