Polyaluminocarbosilane with high aluminum content and low oxygen content, preparation method and SiAlC ceramic

A technology of polyaluminocarbosilane and low oxygen content, which is applied in the field of SiAlC ceramics and polyaluminocarbosilane preparation, can solve the problems of high preparation temperature, low oxygen content and complex reaction of polyaluminocarbosilane, and achieve excellent high temperature resistance and Antioxidant performance, improved preparation efficiency, simple and controllable process

Active Publication Date: 2022-02-08
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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Problems solved by technology

[0005] The object of the present invention is to overcome above-mentioned defect, provide a kind of preparation method of the polyaluminocarbosilane of high aluminum content, low oxygen content, this method adopts liquid hyperbranched liquid polycarbosilane and methyl aluminoxane as raw material, in airtight inert Under certain conditions, hyperbranched liquid polycarbosilane and aluminoxane compound are grafted and copolymerized to prepare polyaluminocarbosilane. By adjusting the ratio of raw materials, the content of aluminum in polyaluminocarbosilane can be adjusted, and the preparation process is simple. , no by-products are produced, and the problems of high preparation temperature and complicated reaction of polyaluminocarbosilane are avoided; the present invention also provides a polyaluminocarbosilane prepared based on the above method, which has high and adjustable aluminum content, low oxygen content, etc. Features, the mass percentage content of aluminum element can be 0-20%, and the mass percentage content of oxygen element is less than 2%. The element composition is adjustable, which can be used to prepare aluminum-containing SiC fibers, high-temperature coatings, fiber reinforcements, and ceramic matrix composite materials;

Method used

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  • Polyaluminocarbosilane with high aluminum content and low oxygen content, preparation method and SiAlC ceramic
  • Polyaluminocarbosilane with high aluminum content and low oxygen content, preparation method and SiAlC ceramic

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preparation example Construction

[0035] High-aluminum content of the present invention, the preparation method polyaluminocarbosilane low oxygen content, comprising the steps of:

[0036] Step 1: an inert gas atmosphere replaced Schlenk reaction vessel, particularly an inert gas is charged into the first reactor was evacuated, was repeated 3 to 5 times. Adding a certain amount of liquid hyperbranched polycarbosilanes, a certain proportion of methyl aluminoxane dissolved in an organic solvent and added dropwise to the reaction vessel and sufficiently stirred to obtain a homogeneous solution evenly; hyperbranched a liquid polycarbosilane with good flow properties, it is liquid at room temperature polycarbosilane;

[0037] Step 2: the above-described homogeneous solution was heated reaction initiating system, to obtain a mixed system containing polyaluminum carbosilane. The reaction temperature is 50 ~ 90 ℃, the reaction time is 2 to 20 hours;

[0038] Step 3: After completion of the reaction system temperature is r...

Embodiment 1

[0045] 1) The air in the Schlenk reactor is replaced with an inert gas, specifically, the reactor is first vacuum, and the inert gas is filled into an inert gas and repeated 3 to 5 times. Ultra-branched liquid allylopolymetin silicone 30g (30 mmol) was added, and 32 g (55 mmol) was added to 25 mol / L methyl aluminoxane, and then added to the reactor, stirred slowly. After uniform, it gave a pale yellow homogeneous solution.

[0046] 2) The above-mentioned homogeneous solution was heated to 80 ° C and held for 6 h.

[0047] 3) After the reaction is completed, the system temperature is reduced to 30 ° C or less, and the vacuum pump is opened, and the solvent is removed, the distillation temperature is 60 ° C, the vacuum is -0.09 ~ -0.1MPa, until the system no longer has a solvent is essential The vacuum is stopped, and the temperature is lowered, and finally obtained light yellow liquid polyuminous carbonilane.

[0048] 4) Place the polyuminous carb silicone in the tube furnace, an...

Embodiment 2

[0051] 1) The air in the Schlenk reactor is replaced with an inert gas, specifically, the reactor is first vacuum, and the inert gas is filled into an inert gas and repeated 3 to 5 times. Ultra-bonded liquid allylopolymetin silicone 30g (30 mmol) was added, 10 g (17 mmol) toluene solution was taken at 25 mol / L methyl aluminoxane, slowly added to the reactor, stirring After uniform, it gave a pale yellow homogeneous solution.

[0052] 2) Heat the above-mentioned homogeneous solution to 70 ° C and heat it for 8 h.

[0053] 3) After the reaction is completed, the system temperature is reduced to 30 ° C or less, and the vacuum pump is opened, and the solvent is removed, the distillation temperature is 60 ° C, the vacuum is -0.09 ~ -0.1MPa, until the system no longer has a solvent is essential The vacuum is stopped, and the temperature is lowered, and finally obtained light yellow liquid polyuminous carbonilane.

[0054] 4) Place the polyuminous carb silicone in the tube furnace, and...

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Abstract

The invention discloses a preparation method of polyaluminocarbosilane with high aluminum content and low oxygen content. Liquid hyperbranched liquid polycarbosilane and methylaluminoxane are adopted as raw materials, polyaluminocarbosilane is prepared under closed inert conditions, and the content of aluminum element in the polyaluminocarbosilane can be adjusted by adjusting the ratio of the raw materials. The invention also discloses the polyaluminocarbosilane prepared based on the method, the mass percentage content of aluminum element can be 0-20%, and the mass percentage content of oxygen element is less than 2%. The invention further discloses SiAlC ceramic obtained after high-temperature cracking of the polyaluminocarbosilane, Si, Al and C elements in the SiAlC ceramic are adjustable in composition, and the SiAlC ceramic has excellent high temperature resistance and oxidation resistance, can be used for preparing an ultrahigh-temperature-resistant C / SiAlC ceramic-based composite material through a PIP method, and can also be used for preparing an ultrahigh-temperature oxidation-resistant coating and fiber.

Description

Technical field [0001] Polyaluminocarbosilane present invention belongs to the technical field for preparing a precursor of silicon carbide, in particular to a low oxygen content in the high aluminum content, and a method for preparing a ceramic SiAlC. Background technique [0002] Polyaluminocarbosilane silicon carbide fibers as the third generation precursor, has been widespread concern by scholars, Tyranno SA fibers produced from the pyrolysis polyaluminocarbosilane fiber is the best known high-temperature properties, the aluminum preparation of silicon carbide ceramic precursor is of great significance. [0003] Currently, the preparation of aluminum-containing preceramic mainly by reaction of the organosilicon polymer and aluminum-containing compounds obtained. According to the state of the silicone polymer, synthetic aluminum-containing preceramic classification may be to use a solid synthetic organic polymer and silicon with liquid silicone polymer synthesis. Initially, Ja...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/56C04B35/622C04B35/80
CPCC08G77/60C04B35/56C04B35/62222C04B35/62277C04B35/80Y02E60/10
Inventor 武婧书胡继东冯志海许艺芬田跃龙李媛齐晨
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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