Synthetic method of trisilylamine

[0023] Example 1

[0024] ‍A method for synthesizing trimethylsilylamine, including the following steps:

[0025] 1) A method for synthesizing trimethylsilylamine using a catalytic distillation tower. The catalytic distillation tower is composed of a rectification section, a reaction section, a stripping section and a tower still connected in sequence from the top of the tower to the bottom of the tower. The preparation method includes the following steps: purging the catalytic distillation tower with inert gas in advance, and simultaneously adding monochlorosilane and ammonia in gaseous form from the rectification section and the stripping section to the catalytic distillation tower for reaction. The molar ratio of chlorosilane and ammonia is 1:1.8, the space velocity of monochlorosilane is 1/h, the reaction pressure is 0.4MPa, and the reaction temperature of the distillation tower is 370℃. The reaction product from the bottom of the tower is continuously drawn, and NH4Cl is separated, and then passed through the industry. Well-known impurity removal and purification technology to obtain high-purity trimethylsilylamine;

[0026] 2) The reaction section is filled with stainless steel corrugated catalytic packing. The preparation method is as follows: add 2 parts of iron palladium nickel carbon fiber to 100 parts of stainless steel corrugated packing by weight, and then wrap the stainless steel corrugated packing with glass fiber cloth to obtain stainless steel Corrugated catalytic packing;

[0027] 3) The preparation method of the iron-palladium-nickel carbon fiber is:

[0028] According to parts by weight, 100 parts of polydimethylsilane are cracked at 460℃ under the protection of high-purity nitrogen to obtain liquid polysilane, and then 0.03 parts of cyclopentadienyl iron and 0.03 parts of dichloro(1,5-ring Octadiene) palladium, 0.05 parts of bis(1,5-cyclooctadiene) nickel, 1 part of azobisisoheptonitrile, 1 part of trans-2-dodecanol, 0.05 parts of 5- Chloro-8-quinoline acrylic acid was reacted for 30 hours, and the product was dissolved in xylene, filtered, and distilled under reduced pressure to obtain polyiron palladium nickel carbosilane. After porous melt spinning, continuous firing at 1600°C under the protection of high-purity nitrogen, iron-palladium-nickel carbon fiber is produced.

[0029] Example 2

[0030] A method for synthesizing trimethylsilylamine, including the following steps:

[0031] 1) A method for synthesizing trimethylsilylamine using a catalytic distillation tower. The catalytic distillation tower is composed of a rectification section, a reaction section, a stripping section and a tower still connected in sequence from the top of the tower to the bottom of the tower. The preparation method includes the following steps: purging the catalytic distillation tower with inert gas in advance, and simultaneously adding monochlorosilane and ammonia in gaseous form from the rectification section and the stripping section to the catalytic distillation tower for reaction. The molar ratio of chlorosilane and ammonia is 1:1.2, the space velocity of monochlorosilane is 0.5/h, the reaction pressure is 0.2MPa, and the reaction temperature of the distillation tower is 350°C. The reaction products from the bottom of the tower are continuously extracted, and NH4Cl is separated, and then passed through the industry. Well-known impurity removal and purification technology to obtain high-purity trimethylsilylamine;

[0032] 2) The reaction section is filled with stainless steel corrugated catalytic packing. The preparation method is as follows: by weight, 1 part of iron-palladium-nickel carbon fiber is added to the gap of 100 parts of stainless steel corrugated packing, and then the stainless steel corrugated packing is wrapped with glass fiber cloth to obtain stainless steel Corrugated catalytic packing;

[0033] 3) The preparation method of the iron-palladium-nickel carbon fiber is:

[0034] According to parts by weight, 100 parts of polydimethylsilane are cracked at 400°C under the protection of high-purity nitrogen to obtain liquid polysilane, and then 0.01 parts of cyclopentadienyl iron and 0.01 parts of dichloro (1,5-ring Octadiene) palladium, 0.01 parts of bis(1,5-cyclooctadiene) nickel, 0.5 parts of azobisisoheptonitrile, 0.5 parts of trans-2-dodecanol, 0.01 parts of 5- Chloro-8-quinoline acrylic acid was reacted for 10 hours, the product was dissolved in xylene, filtered, and distilled under reduced pressure to obtain polyiron palladium nickel carbosilane. Through porous melt spinning and continuous firing under the protection of high-purity nitrogen at 1000°C, iron-palladium-nickel carbon fiber is produced.

[0035] Example 3

[0036] A method for synthesizing trimethylsilylamine, including the following steps:

[0037] 1) A method for synthesizing trimethylsilylamine using a catalytic distillation tower. The catalytic distillation tower is composed of a rectification section, a reaction section, a stripping section and a tower still connected in sequence from the top of the tower to the bottom of the tower. The preparation method includes the following steps: purging the catalytic distillation tower with inert gas in advance, and simultaneously adding monochlorosilane and ammonia in gaseous form from the rectification section and the stripping section to the catalytic distillation tower for reaction. The molar ratio of chlorosilane and ammonia is 1:3, the space velocity of monochlorosilane is 2/h, the reaction pressure is 1MPa, and the reaction temperature of the distillation tower is 420℃. The reaction products from the bottom of the tower are continuously drawn out, and NH4Cl is separated. High purity trimethylsilyl amine can be obtained by the refined technology of removing impurities;

[0038] 2) The reaction section is filled with stainless steel corrugated catalytic packing. The preparation method is as follows: add 10 parts of iron-palladium-nickel carbon fiber to 100 parts of stainless steel corrugated packing by weight, and then wrap the stainless steel corrugated packing with glass fiber cloth to obtain stainless steel Corrugated catalytic packing;

[0039] 3) The preparation method of the iron-palladium-nickel carbon fiber is:

[0040] According to parts by weight, 100 parts of polydimethylsilane are cracked at 500°C under the protection of high-purity nitrogen to obtain liquid polysilane, and then 0.1 parts of cyclopentadienyl iron and 0.1 parts of dichloro (1,5-ring Octadiene) palladium, 0.1 part of bis(1,5-cyclooctadiene) nickel, 2 parts of azobisisoheptonitrile, 2 parts of trans-2-dodecanol, 0.1 part of 5- Chloro-8-quinoline acrylic acid, reacted for 40 hours, the product was dissolved in xylene, filtered, and distilled under reduced pressure to obtain polyiron-palladium-nickel-carbosilane, which was continuously sintered at 1800°C under the protection of high-purity nitrogen and porous melt spinning The iron-palladium-nickel carbon fiber is produced.