1,2-Ethanediamine, N,N-bis3-(trimethoxysilyl)propyl- synthesis

Yield:74956-86-8 752.8 g

Reaction Conditions:

at 130; for 7.5 h;

Steps:

2

According to 1:2 of the feed ratio, First, 2 mol (397.4 g) The chloropropyltrimethoxysilane feedstock is taken into a metering tank, A further 4 mol (889.6 g) N-(2-aminoethyl)-3-aminopropyltrimethoxysilane feed into the reactor, 90 rpm The stirrer was raised to 130 °C under stirring. After the kettle temperature rose to 130 °C, The use of dropping funnel drop way, The chloropropyltrimethoxysilane in the metering tank was added dropwise to the autoclave over 3.5 hours, and the reaction was continued for 4 hours at 130 °C after completion of the dropwise addition. After 4 hours of incubation reaction, the kettle temperature was reduced to below 40 °C and the filter was filtered according to a conventional process. The resulting residue was washed with 400 g of petroleum ether, To give by-product N-(2-aminoethyl)-3-aminopropyltrimethoxysilane hydrochloride 525.3 g, the resulting filtrate and the washing solution were mixed, obtained: 1151.1 g of crude bis [3-(trimethoxysilyl)propyl]ethylenediamine, The crude product is vacuum distilled in a conventional process, To distill off the residual petroleum ether in the wash solution, obtained: 752.8 g of bis(3-(trimethoxysilyl)propyl]ethylenediamine, GC detection content of 93.8%, product quality yield of 58.5%.

References:

CN104140437,2016,B Location in patent:Paragraph 0026; 0027