Room temperature curing agent for high-temperature-resistant organosilicon materials, preparation method and applications thereof

A room temperature curing agent and silicone technology, applied in the field of room temperature curing agents, can solve the problems of small contact probability of reaction raw materials, increase material cost, unstable product structure, etc., and achieve mass transfer and heat transfer control and increase contact area. and time, the effect that is beneficial to the mass transfer process

Active Publication Date: 2019-04-02
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used method at present is to introduce large-volume anti-degradation components into the molecular weight structure of organic silicon, such as cyclodisilazane, carborane, etc., while effectively improving the temperature resistance of organic silicon materials, it greatly increases The cost of materials; another method is to add a large amount of heat-resistant inorganic fillers, which can effectively improve the temperature resistance of organic silicon materials and often lead to poor processability, which limits the application of materials
[0003] Existing silicone protective materials usually need to be cured at high temperature, and the curing temperature is generally above 150°C, which is inconvenient for construction and consumes a lot of energy, which is not conducive to industrial application and promotion
In addition, at present, chlorosilanes are mostly used to directly pass ammonia gas to prepare polysilazane curing agents. The contact probability of the reaction raw materials is small, and the ammonium chloride generated during the reaction will coat the reaction raw materials. The utilization rate of raw materials is insufficient, and the reaction process is difficult to control. , the product structure is unstable; and because the ammonolysis rate of multifunctional chlorosilanes is often much higher than that of difunctional chlorosilanes, it is easy to have too many multifunctional structures such as trifunctionality in the product, the viscosity of the curing agent is large, and the cured organic Silicon material is too hard to meet the needs of practical applications

Method used

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  • Room temperature curing agent for high-temperature-resistant organosilicon materials, preparation method and applications thereof
  • Room temperature curing agent for high-temperature-resistant organosilicon materials, preparation method and applications thereof
  • Room temperature curing agent for high-temperature-resistant organosilicon materials, preparation method and applications thereof

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preparation example Construction

[0039] The preparation method of the present invention will be further described in detail in conjunction with specific examples below. It should be understood that the following examples are only for illustrating and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies realized based on the above contents of the present invention are covered within the scope of protection intended by the present invention.

[0040] The experimental methods used in the following examples are conventional methods unless otherwise specified;

[0041] The reagents and materials in the following examples can be obtained from commercial sources unless otherwise specified.

Embodiment 1

[0043] 600L of petroleum ether (boiling point 30-60°C) was dried through molecular sieves and added into a 1000L reactor through a metering pump, and 100kg of dimethyldichlorosilane and 60kg of methyltrichlorosilane were added to the reactor through the frequency control of the metering pump. Silane, start the stirring of the reactor at 5000rpm, control the temperature in the reactor at -20°C through a refrigerator, dry the ammonia gas through a molecular sieve, and then enter the reactor through mass flow meter control, and pass through 5 inlets arranged around the stirring shaft. The pores enter the reaction system in the form of microbubbles under the air pressure of 3MPa. 10kg of ceramic balls are placed in the reactor to break the ammonium chloride p-dimethyldichlorosilane and methyltrichlorosilane produced in situ. And the resulting polymethylsilazane coating. After 24 hours, no ammonia gas can be detected in the tail gas, and the reaction system stops passing ammonia. D...

Embodiment 2

[0048] Put 1200L of ethylene glycol dimethyl ether into a 2000L reactor through a metering pump after drying through molecular sieves, add 200kg of diphenyldichlorosilane and 200kg of phenyltrichlorosilane into the reactor through the frequency control of the metering pump, and start The stirring of the reaction kettle is at 8000rpm, and the temperature inside the reaction kettle is controlled at 80°C by heating. The ammonia gas is dried through molecular sieves and then controlled by a mass flow meter to enter the reaction kettle. There are 10 air inlet holes arranged around the stirring shaft at a temperature of 10MPa. Under the assistance of air pressure, it enters the reaction system in the form of microbubbles. 30kg of ceramic balls are placed in the reactor to break the ammonium chloride p-diphenyldichlorosilane, phenyltrichlorosilane and polyphenylene chloride generated in situ. Coating with silazane. The reaction system stopped passing ammonia after 16 hours when no am...

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Abstract

The invention provides a room temperature curing agent for high-temperature-resistant organosilicon materials, a preparation method and applications thereof. The room temperature curing agent comprises polysilazane and a catalyst, wherein the molecular structure of the polysilazane is optimized, and only contains difunctional Si-N chain segments and trifunctional Si-N chain segments, and the random branched structure is formed by a polymerization reaction; by adjusting the feeding ratio, pressurizing during the aminolysis and using ceramic ball-assisted mass transfer, the use amounts of the trifunctional silane and the ammonia gas for forming the trifunctional Si-N chain segment with the same content are substantially reduced, the molecular structure of the polysilazane is optimized, the generation of ammonium chloride is reduced, and the mass transfer and heat transfer control during the aminolysis is easily achieved; and the optimization does not affect the formation of the cross-linked network of the cured organosilicon material, and the structure optimizing meets the development trend of green chemistry.

Description

technical field [0001] The invention relates to a room-temperature curing agent for a high-temperature-resistant organic silicon material, a preparation method and an application thereof, and belongs to the field of high-temperature-resistant materials and their preparation. Background technique [0002] With the rapid development of modern aerospace requirements, the flight speed of the required aircraft is getting faster and faster, which makes the temperature of the aircraft face higher and higher, which puts forward higher and higher requirements for high temperature resistant protective materials, such as Room temperature curing, high temperature resistance, high mechanical properties of protective materials. Because of its good heat resistance, cold resistance, weather resistance, aging resistance and other characteristics, silicone materials are widely used as material substrates resistant to high temperatures of 250 ° C, but at higher operating temperatures above 350...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62C08G77/06C08G77/08C08G77/34C08L83/04C08L83/16C08K3/36
CPCC08G77/06C08G77/08C08G77/34C08G77/62C08G77/80C08L83/04C08L2205/02C08L83/16C08K3/36
Inventor 张学忠张志杰谢择民谭永霞汪倩赵建玉张学孝
Owner INST OF CHEM CHINESE ACAD OF SCI
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