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Synthesis device and synthesis method of electronic-grade tri (dimethylamino) silane

A technology of dimethylamino and synthesis equipment, which is applied in the direction of separation methods, silicon organic compounds, chemical instruments and methods, etc., can solve the problems of hidden safety hazards, high reaction costs, difficult control of reaction temperature, etc., and achieve reduction of process costs and reduction of The effect of rapid fluctuations in reaction temperature and stable temperature

Active Publication Date: 2021-12-17
CHINA SILICON CORP LTD +1
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Problems solved by technology

[0006] The main purpose of the present invention is to provide a synthesis device and synthesis method of electronic grade tris(dimethylamino)silane, to solve the problem of reaction temperature in existing synthesis methods It is difficult to control and respond to problems with high cost and potential safety hazards

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  • Synthesis device and synthesis method of electronic-grade tri (dimethylamino) silane

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preparation example Construction

[0033] As described in the background art, the existing electronic-grade tris(dimethylamino)silane synthesis method has the problems of difficult control of reaction temperature, high reaction cost and potential safety hazards. In order to solve the above technical problems, such as figure 1As shown, the application provides a synthetic device for electronic-grade tris(dimethylamino)silane, which includes: a raw material premixing device 100, a reaction device 210 and a pressurizing device 300 and purification unit 400. The raw material premixing device 100 is provided with a chlorine receiving agent inlet 101, a dimethylammonium chloride inlet 102, a solvent inlet 103 and a mixed solution outlet 104; the reaction device 210 is provided with an inert atmosphere inlet 212, a mixed solution inlet 213, and a trichlorosilane inlet 211 and the crude product outlet 214, the mixed solution inlet 213 is communicated with the mixed solution outlet 104 and arranged; The pressurizing de...

Embodiment 1

[0063] A novel aminosilane and preparation method thereof, comprising the following steps: first, in N 2 Under protection, add 16.25g (0.25mol) zinc powder, 30ml n-heptane, 23.85g (0.3mol) chlorodimethylamine solution to the stirred bed reactor, start the mechanical stirring for 15min, slowly add 13.6 g (0.1mol) trichlorosilane, continue to stir and react, control the temperature at 85±2°C, and the pressure inside the kettle at 65KPa, after 2 hours of reaction, filter in turn (manufacturer: Yantai Jianghai Filtration Equipment Co., Ltd. model JHDS series filter) , one-stage rectification (the pressure of the tower kettle is 125Kpa, the temperature of the tower top is 145-148°C, the reflux feed ratio is 17, and the number of theoretical plates is 115), combined adsorption (the complexing agent is Hubei Yuancheng Saichuang Technology Co., Ltd. Industrial-grade sodium ethylenediamine tetramethylene phosphonate with a purity of 99% produced by the company; the molecular sieve is 1...

Embodiment 2

[0065] A novel aminosilane and preparation method thereof, comprising the following steps: first, in N 2 Under protection, add 7.8g (0.3mol) of aluminum powder, 40ml of n-heptane, 27.83g (0.35mol) of chlorodimethylamine solution to the stirred bed reactor, start the mechanical stirring for 15min, and slowly add 13.6 g (0.1mol) trichlorosilane, continue to stir and react, control the temperature at 85±2°C, and the pressure inside the kettle at 70KPa, after 2 hours of reaction, filter in turn (manufacturer: Yantai Jianghai Filtration Equipment Co., Ltd. model JHDS series filter) , one-stage rectification (the pressure of the tower kettle is 125Kpa, the temperature of the tower top is 145-148°C, the reflux feed ratio is 17, and the number of theoretical plates is 115), combined adsorption (the complexing agent is Hubei Yuancheng Saichuang Technology Co., Ltd. Industrial-grade sodium ethylenediamine tetramethylene phosphonate with a purity of 99% produced by the company; the molec...

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Abstract

The invention provides a synthesis device and a synthesis method of electronic-grade tri (dimethylamino) silane. The synthesis device of the electronic-grade trisilane comprises a raw material premixing device, a reaction unit, a pressurizing device and a purification unit, wherein the raw material premixing device is provided with a chlorine receiving agent inlet, a dimethylamine chloride inlet, a solvent inlet and a mixed liquid outlet; the reaction unit is provided with an inert atmosphere inlet, a mixed liquid inlet, a trichlorosilane inlet and a crude product outlet, and the mixed liquid inlet is communicated with the mixed liquid outlet; the pressurizing device is used for adjusting the pressure in the reaction unit; and the purification unit is provided with a purification inlet and a discharge port, and the purification inlet is communicated with the crude product outlet through a crude product conveying pipeline. The synthesis device is adopted to change the types of the reaction raw materials and the feeding mode, and meanwhile, the pressurizing device is arranged, so that the fluctuation of the reaction temperature in the reaction device can be reduced, and the process cost is reduced.

Description

technical field [0001] The invention relates to the field of synthesis of electronic-grade tris(dimethylamino)silane, in particular to a synthesis device and method for electronic-grade tris(dimethylamino)silane. Background technique [0002] The size of MOS transistors in basic devices in VLSI continues to shrink, when SiO 2 When the thickness of the gate dielectric is reduced to the nanometer level, through SiO 2 The leakage current increases exponentially with decreasing thickness. The above-mentioned huge leakage current not only seriously affects the device performance, but also eventually leads to SiO 2 Can not play an insulating role. Use high dielectric constant (i.e. high-K materials) instead of SiO 2 It is currently the most promising way to solve this problem. The use of high-K materials can maintain the same capacitance density on the one hand, and on the other hand, it can also make the gate dielectric have a larger physical thickness, thereby avoiding the ...

Claims

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Application Information

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IPC IPC(8): B01D3/00C07F7/02
CPCB01D3/009C07F7/025Y02P20/10
Inventor 贺玉刚常欣王芳万烨赵雄孙强赵喜哲李圆晓
Owner CHINA SILICON CORP LTD
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