A kind of silane compound containing oxygen and nitrogen heterocycle, its preparation method and application, and olefin polymerization method
A technology for silane compounds and nitrogen heterocyclic compounds, applied in the field of olefin polymerization, can solve the problems of harsh operating conditions, bumping, explosion, etc., and achieve the effects of low product cost, easy availability of raw materials and mild reaction conditions
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[0065] According to a preferred embodiment of the present invention, the preparation method of the silane compound containing oxygen nitrogen heterocyclic ring adopts the following steps: 2 Under protective conditions, in an aprotic solvent, add morpholine to the reaction flask in sequence, and stir evenly; under the condition of preferably 0-10°C, add n-butyllithium-n-hexane solution dropwise, the n-butyl Lithium-n-hexane solution is a commercially available reagent; then add the siloxane compound shown in formula (III) dropwise; centrifuge the reaction solution after the reaction, wash twice with the above-mentioned aprotic solvent, collect the filtrate, and use The above-mentioned aprotic solvent was evaporated by a rotary evaporator, and distilled under reduced pressure to collect fractions.
[0066] According to another preferred embodiment of the present invention, the preparation method of the silane compound containing oxygen nitrogen heterocyclic ring adopts the follo...
Embodiment 1
[0074] Preparation of bismorpholinodimethoxysilane according to the invention
[0075] in N 2 Under protective conditions, 0.916 g of morpholine and 10 ml of n-hexane were successively added to the reaction flask, and stirred. At a temperature of 5°C, add 4.2ml (2.87M) butyllithium-n-hexane solution dropwise for 30 minutes; after 30 minutes, add 0.85 g of tetramethoxysilane dropwise to the reaction solution to continue the reaction 6h. The reaction solution was separated by centrifugation, the precipitate was washed twice with n-hexane, and the filtrate was collected. Evaporate the n-hexane solvent with a rotary evaporator, distill under reduced pressure, collect the 84°C / 80Pa fraction, weigh 0.88g, and have a content of 99.0% (GC), carry out nuclear magnetic resonance testing, and obtain the following peaks:
[0076] 1 HNMR (CDCl 3 / TMS, 300MHz) δ (ppm): 2.99 (t, 8H, 4CH 2 ), 3.51(s, 6H, 2OCH 3 ), 3.58(t, 8H, 4CH 2 )
Embodiment 2
[0078] Preparation of pyrrolylmorpholinodimethoxysilanes according to the invention
[0079] in N 2 Under protective conditions, 4.58 g of pyrrolidine and 50 ml of n-hexane were successively added into the reaction flask, and stirred. At a temperature of 10° C., 25.4 ml (2.5 M) of butyllithium-n-hexane solution was added dropwise for 30 minutes. After 1 hour, 13.4 g of tetramethoxysilane was added dropwise to the reaction liquid, and the reaction was continued for 17 hours. The reaction solution was separated by centrifugation, the precipitate was washed twice with n-hexane, and the filtrate was collected. Evaporate the n-hexane solvent with a rotary evaporator, and distill under reduced pressure to collect a fraction at 86-91°C / 90Pa, which is called intermediate A2, weighing 7.7g, and having a content of 99.0% (GC).
[0080] in N 2 Under protective conditions, 1.58 g of morpholine and 20 ml of n-hexane were successively added to the reaction flask, and stirred. At a temp...
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