Preparation method of di(diethylamino)silane

Abstract

The invention provides a preparation method of di(diethylamino)silane. The method comprises the following steps: step 1, adding an alkane CnH(2n+2) (n>=5) solution of n-butyllithium into a reactor protected by inert atmosphere, dropwise adding diethylamine for a reaction while performing stirring, maintaining the temperature of the reaction system in a range from -60 DEG C to -30 DEG C, and performing stirring for reaction for 10-15 h; step 2, pumping dichlorosilane in at a temperature in a range from -60 DEG C to -30 DEG C, performing stirring for reaction for 15-20 h while maintaining the temperature in a range from -60 DEG C to -30 DEG C, increasing the temperature to a room temperature, and evaporating alkane CnH(2n+2) (n>=5) under a normal pressure; and step 3, performing vacuum distillation to make a coarse di(diethylamino)silane product out. The coarse di(diethylamino)silane product is subjected to vacuum distillation to obtain di(diethylamino)silane with high purity. The preparation method has the beneficial effects that the selected reagents are free of toxicity, thereby ensuring safety of operators; the reaction process is relatively mild and has no potential safety hazard; and the reaction efficiency is very high.

Description

technical field

[0001] The invention relates to a preparation method of bis(diethylamino)silane, which belongs to the field of chemical industry. Background technique

[0002] Silicon nitride film is a multifunctional material with excellent properties such as low dielectric constant, high insulation, low leakage point, and oxidation resistance. As an efficient device surface passivation layer, silicon nitride film is widely used in semiconductor device technology; silicon nitride film is also used in the integrated circuit industry as interlayer insulation, dielectric capacitance and wear-resistant and anti-corrosion coating; In silicon-based solar cells, silicon nitride films are used as passivation films and anti-reflection films. At the same time, silicon nitride thin films have excellent mechanical properties and good stability, and are more and more widely used in the nascent micro-processing technology.

[0003] In addition to excellent mechanical and physical prope...

Examples

Embodiment 1

[0020] Under a nitrogen atmosphere, 5000 ml of n-butyllithium in n-hexane solution was added to the reaction kettle with a concentration of 2.5 moles per liter. Under the condition of stirring, add 1000 grams of diethylamine dropwise to the reaction kettle, control the rate of dropping to prevent the influence on the temperature of the system, so as to keep the temperature in the kettle at -60°C, and keep the temperature in the kettle at -60°C after the dropwise addition. °C and stirred for 15 hours. Then 690 g of dichlorosilane was introduced, and the rate of introduction was controlled to keep the temperature in the kettle at -60°C. Finally, the mixture was stirred and reacted at -60°C for 15 hours, and then rose to room temperature. The solvent n-hexane was distilled off under normal pressure, and then bis(diethylamino)silane was distilled off under reduced pressure. The rectification pressure was 15mmHg, and the rectification temperature was 70°C. 990 g of the product wer...

Embodiment 2

[0022] Under an argon atmosphere, add 5000ml of n-butyllithium-n-hexane solution to the reaction kettle, the concentration is 2.5 moles per liter, and under stirring conditions, add 920 grams of diethylamine dropwise to the reaction kettle, and control the dropwise Speed, keep the temperature in the kettle at -45°C, keep stirring at -45°C for 10 hours after the dropwise addition, and then feed 630 grams of dichlorosilane at a speed to keep the inside of the kettle at -45°C, and finally at -45°C After stirring the reaction for 12 hours, it was allowed to warm to room temperature. The solvent n-hexane was distilled off under normal pressure, and then bis(diethylamino)silane was distilled off under reduced pressure. The rectification pressure was 15mmHg, and the rectification temperature was 70°C. 905 g of the product were obtained, and the yield (mole weight ratio relative to silicon) was 83.2%.

Embodiment 3

[0024] Under a nitrogen atmosphere, 5000 ml of n-butyllithium in n-hexane solution was added to the reaction kettle with a concentration of 2.5 moles per liter. Under the condition of stirring, add 1000 grams of diethylamine dropwise to the reaction kettle, control the rate of dropping to prevent affecting the temperature of the system, so as to keep the temperature in the kettle at -30°C, and keep the temperature in the kettle at -30°C after the dropwise addition , stirred for 12 hours. Then 690 g of dichlorosilane was introduced, and the rate of introduction was controlled to keep the temperature in the kettle at -30°C. Finally, the mixture was stirred and reacted at -30°C for 10 hours, and then rose to room temperature. The solvent n-hexane was distilled off under normal pressure, and then bis(diethylamino)silane was distilled off under reduced pressure. The rectification pressure was 15mmHg, and the rectification temperature was 70°C. 973 g of the product were obtained, a...

technical field

[0001] The invention relates to a preparation method of bis(diethylamino)silane, which belongs to the field of chemical industry. Background technique

[0002] Silicon nitride film is a multifunctional material with excellent properties such as low dielectric constant, high insulation, low leakage point, and oxidation resistance. As an efficient device surface passivation layer, silicon nitride film is widely used in semiconductor device technology; silicon nitride film is also used in the integrated circuit industry as interlayer insulation, dielectric capacitance and wear-resistant and anti-corrosion coating; In silicon-based solar cells, silicon nitride films are used as passivation films and anti-reflection films. At the same time, silicon nitride thin films have excellent mechanical properties and good stability, and are more and more widely used in the nascent micro-processing technology.

[0003] In addition to excellent mechanical and physical prope...

Examples

Embodiment 1

[0020] Under a nitrogen atmosphere, 5000 ml of n-butyllithium in n-hexane solution was added to the reaction kettle with a concentration of 2.5 moles per liter. Under the condition of stirring, add 1000 grams of diethylamine dropwise to the reaction kettle, control the rate of dropping to prevent the influence on the temperature of the system, so as to keep the temperature in the kettle at -60°C, and keep the temperature in the kettle at -60°C after the dropwise addition. °C and stirred for 15 hours. Then 690 g of dichlorosilane was introduced, and the rate of introduction was controlled to keep the temperature in the kettle at -60°C. Finally, the mixture was stirred and reacted at -60°C for 15 hours, and then rose to room temperature. The solvent n-hexane was distilled off under normal pressure, and then bis(diethylamino)silane was distilled off under reduced pressure. The rectification pressure was 15mmHg, and the rectification temperature was 70°C. 990 g of the product wer...

Embodiment 2

[0022] Under an argon atmosphere, add 5000ml of n-butyllithium-n-hexane solution to the reaction kettle, the concentration is 2.5 moles per liter, and under stirring conditions, add 920 grams of diethylamine dropwise to the reaction kettle, and control the dropwise Speed, keep the temperature in the kettle at -45°C, keep stirring at -45°C for 10 hours after the dropwise addition, and then feed 630 grams of dichlorosilane at a speed to keep the inside of the kettle at -45°C, and finally at -45°C After stirring the reaction for 12 hours, it was allowed to warm to room temperature. The solvent n-hexane was distilled off under normal pressure, and then bis(diethylamino)silane was distilled off under reduced pressure. The rectification pressure was 15mmHg, and the rectification temperature was 70°C. 905 g of the product were obtained, and the yield (mole weight ratio relative to silicon) was 83.2%.

Embodiment 3

[0024] Under a nitrogen atmosphere, 5000 ml of n-butyllithium in n-hexane solution was added to the reaction kettle with a concentration of 2.5 moles per liter. Under the condition of stirring, add 1000 grams of diethylamine dropwise to the reaction kettle, control the rate of dropping to prevent affecting the temperature of the system, so as to keep the temperature in the kettle at -30°C, and keep the temperature in the kettle at -30°C after the dropwise addition , stirred for 12 hours. Then 690 g of dichlorosilane was introduced, and the rate of introduction was controlled to keep the temperature in the kettle at -30°C. Finally, the mixture was stirred and reacted at -30°C for 10 hours, and then rose to room temperature. The solvent n-hexane was distilled off under normal pressure, and then bis(diethylamino)silane was distilled off under reduced pressure. The rectification pressure was 15mmHg, and the rectification temperature was 70°C. 973 g of the product were obtained, a...